CN105942431A - Sea salt and folium isatidis extract containing plant salt and method for preparing plant salt by using heavy metal ion removal process through nanofiber membrane - Google Patents

Sea salt and folium isatidis extract containing plant salt and method for preparing plant salt by using heavy metal ion removal process through nanofiber membrane Download PDF

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CN105942431A
CN105942431A CN201610282891.3A CN201610282891A CN105942431A CN 105942431 A CN105942431 A CN 105942431A CN 201610282891 A CN201610282891 A CN 201610282891A CN 105942431 A CN105942431 A CN 105942431A
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salt
nano fibrous
fibrous membrane
content
plant salt
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王胜
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/44Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/44Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/442Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • C02F2101/203Iron or iron compound
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00General aspects of water treatment
    • C02F2301/08Multistage treatments, e.g. repetition of the same process step under different conditions

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention provides sea salt and folium isatidis extract containing plant salt. In the plant salt, the content of NaCl is 75%-85%, the content of isatan B is 0.5%-1.5%, the content of beta-sitosterol is 0.1%-0.5% and the content of palmitic acid is 0.6%-0.8%. The invention also provides a method for preparing the plant salt by using a heavy metal ion removal process through a nanofiber membrane. The method comprises the step of preparing refined brine; the step of preparing the refined brine includes the sub-step of removing heavy metal ions with the nanofiber membrane; the sub-step of removing heavy metal ions with the nanofiber membrane includes the step of preparing a PAN (Polyacrylonitrile) spinning solution, wherein the nanofiber membrane has 3-5 layers and the filtration pressure is controlled at 0.1-0.5 MPa. The sea salt and folium isatidis extract containing plant salt prepared by the invention does not cake after being placed for three years and has the obvious effect on promotion of wound healing.

Description

A kind of containing sea salt and the plant salt of Folium Isatidis extract and use nano fibrous membrane except weight Metal ion technique prepares the method for plant salt
Technical field
The present invention relates to the evaluation and exploration technology of plant salt in plant, specifically one carries containing sea salt and Folium Isatidis The plant salt taking thing and the method using nano fibrous membrane removing heavy metals ion processes to prepare plant salt.
Background technology
The mankind rely on sea water to evaporate brine and the method such as well salt, rock salt mining manufactures Sal for a long time, meet self-demand.But The salt that the mankind are eaten for a long time is substantially inorganic matter, can only meet the human body self demand to inorganic salt, it is difficult to adapt to due to Living standard promotes the mankind the caused demand to several functions food, and Sal is essentially sodium chloride the most in the market, Too high Na+ takes in the blood pressure to human body, blood fat etc. all significantly negative effect.This problem be there has been relatively by people at present Deep understanding, produces the products such as Cardia Salt, but these products is still in the production of inorganic stage, it is impossible to meet the mankind further Absorption to aminoacid, protein and multivitamin and trace element requires and to fat-reducing, blood fat reducing, anti-ageing hope of waiting for a long time Demand.
Based on case above, current India takes the lead in utilizing Salicornia Bigelovii Torr. to produce plant salt in the world, it was reported that this plantation Thing salt, rich in trace element such as potassium, calcium, magnesium, ferrum, without adding any chemical substance in the course of processing, therefore can be rated as " natural battalion Support salt ".The sample of this edible salt has been sent to more overseas companies and has carried out business potential assessment, and the preliminary feedback obtained makes us bulging Dance.
But in the prior art, produce during plant salt, be primarily present following deficiency:
1, in the Sal produced, NaCl content is high, and long-term a large amount of edible serious harm people's is healthy;
2, utilizing the Sal that coastal making from brine is standby in prior art, content of beary metal is higher;
3, in the test produced, Folium Isatidis composition is not contained;
4, in prior art, the edible salt of preparation, do not contain specific Chinese medicinal ingredients, do not have functional;
5, edible salt prepared by prior art, easily lumps.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, it is provided that one is extracted containing sea salt and Folium Isatidis The method that the plant salt of thing and employing nano fibrous membrane removing heavy metals ion processes prepare plant salt, to reach following invention mesh :
1, in the plant salt containing sea salt and Folium Isatidis extract prepared by the present invention, NaCl content is low, possibly together with more multi-functional one-tenth Part, body health benefits can be eaten for a long time;
2, the plant salt content of beary metal containing sea salt and Folium Isatidis extract that prepared by the present invention is relatively low;
3, the plant salt containing sea salt and Folium Isatidis extract prepared by the present invention contains Folium Isatidis composition;
4, the present invention prepare containing sea salt and the plant salt of Folium Isatidis extract, prevented from caking;
5, the present invention prepare containing sea salt and the plant salt of Folium Isatidis extract, there is the effect promoting wound healing.
To achieve the above object of the invention, the technical solution used in the present invention is as follows:
It is a kind of containing sea salt with the plant salt of Folium Isatidis extract, it is characterised in that: containing sea salt in described plant salt, described plant salt It it is light brown.
NaCl content: 72-80% in described plant salt, moisture: 1-3%, MgCl2Content: 0.01-0.05%, CaSO4 Content: 0.05-0.1%, isatan B content: 0.5-1.5%, cupreol content: 0.1-0.5%, palmitic acid content: 0.6- 0.8%, molybdenum ion content≤0.03mg/kg, silver ion content≤0.04mg/kg, cobalt ion content≤0.05mg/kg.
A kind of method using nano fibrous membrane removing heavy metals ion processes to prepare plant salt, it is characterised in that: include essence Causing salt preparation process, described exquisite salt preparation process includes nano fibrous membrane removing heavy metals step, described nano fibrous membrane Removing heavy metals step includes PAN spinning liquid preparation process, and the number of plies of described nano fibrous membrane is 3-5 layer, and filter pressure controls 0.1-0.5MPa。
Described PAN spinning liquid preparation process, spinning liquid preparation need to add ammonia.
The concentration of the ammonia of described addition is 15-25%.
After adding ammonia, incorporation time is: 2-4h, and temperature controls: 10-15 DEG C.
Described nano fibrous membrane removing heavy metals step also includes spinning process, and spinning nozzle is flat type hole, and spinneret orifice is transversal Face length-width ratio is 4:1.
Described nano fibrous membrane removing heavy metals step also includes amidoxim step;Described amidoxim step is by PAN Nano fibrous membrane is immersed in the alkaline solution containing oxammonium hydrochloride. process.
The pH value of described hydroxylamine hydrochloride solution is 8-11.
Use ammonia regulation hydroxylamine hydrochloride solution pH value.
The reaction temperature of described amidoxim is 110-145 DEG C.
Owing to have employed technique scheme, what the present invention reached has the beneficial effect that:
1, the Herba suadeae glaucae salt sodium chloride content containing sea salt that prepared by the present invention is relatively low, and NaCl content is 72-80%;
2, use the present invention prepare containing sea salt and the plant salt of Folium Isatidis extract, its heavy metal ion content is low, molybdenum ion Content≤0.03mg/kg, silver ion content≤0.04mg/kg, cobalt ion content≤0.05mg/kg;
3, in the plant salt containing sea salt and Folium Isatidis extract prepared by the present invention, isatan B content: 0.5-1.5%, β-paddy steroid Alcohol content: 0.1-0.5%, palmitic acid content: 0.6-0.8%;
4, the present invention prepare containing sea salt and the plant salt of Folium Isatidis extract, place to reach 3 years and do not lump;
5, plant salt prepared by the present invention, have an effect being obviously promoted wound healing, respectively to white mouse, white rabbit, Mini-musk swine In test, in wound depth 5mm, three days wound healing rate >=75%.
Detailed description of the invention
Embodiment 1: containing sea salt and the preparation of the plant salt of Folium Isatidis extract
Step 1, exquisite making from brine are standby
(1) brine collection
Potassium ferrocyanide is added pH value be 7 refined after saturated bittern in, the potassium ferrocyanide being prepared as 0.2 mg/L is molten Liquid, adds sodium carbonate and calcium chloride, stirs, stands, precipitates, remove in salt most Ca2+, Mg2+, Fe2+ etc. from Son, obtains the purest salt.In salt, molybdenum ion content is at 10mg/L, silver ion content 10mg/L, cobalt ion after testing Content 15mg/L.
(2) filter
Mechanical filter: the salt gathered is removed bulky grain solid impurity therein and mechanicalness impurity through mechanical filter;The One layer is that activated alumina is as filtrate, the specification of filter material of described first time filtrate as filtrate, second layer selection quartz sand 2mm, specification 4mm of second layer filtrate, filter type is for filter up and down, and after double medium filtration, the turbidity of salt is less than 5NTU.
Filter-cloth filtering: again by microfiltration cloth filter plate water outlet after mechanical filter, microfiltration cloth filter plate surface covers microfiltration cloth, its material Matter is filter felt or filter cotton, filtering accuracy 25 μm;It filters filtering velocity and controls at 6m/h, and filter pressure is 0.6MPa.
Nanofiltration: the salt after filtering carries out nanofiltration process, and nanofiltration temperature to control at 25 DEG C, adds reducing agent Jiao's sulfurous Acid sodium.The addition of reducing agent is the 20-35% of NF membrane quality.Reducing agent is configured to the solution of 3%, and NF membrane precision controlling exists 7 μm, the material of NF membrane is aromatic polyamides composite.
(3) nano fibrous membrane removing heavy metals
After filtering, clean salt, is filtered by sea water bittern nano fibrous membrane, removes heavy metal ion.Nano fibrous membrane The number of plies be 3 layers, filter pressure control 0.2MPa.The manufacture method of described nano fibrous membrane is:
Prepared by PAN spinning liquid: dimethyl fumarate and 2-methyl-2 pyrrolidone solution are mixed, dissolved by PAN, solution temperature 50 DEG C, adding ammonia after cooling, the concentration of ammonia is 15%, and the addition of ammonia and 2-methyl-2 ketopyrrolidine volume ratio are 2: 1, mix 2h, temperature controls 11 DEG C, is made into spinning solution;Dimethyl fumarate concentration is 20wt.%, 2-methyl-2 ketopyrrolidine Concentration is 23wt.%.
Spinning: by electrostatic spinning process, PAN nano wire is deposited on polyethylene terephthalate non-woven fabrics, obtain It is able to the nano fibrous membrane that polyethylene terephthalate non-woven fabrics is substrate;Spinning voltage is 15kV, relative humidity 35%- 50%;Spinning nozzle is flat type hole, and spinneret orifice cross-sectional aspect ratio is 4:1;The thickness of non-woven fabrics is 1000 μm;PAN nano wire Thickness be 300 μm, PAN nano wire mass content in nano fibrous membrane is 10%.
Amidoxim: PAN nanofiber membrane be immersed in the alkaline solution containing oxammonium hydrochloride., controls oxammonium hydrochloride. molten Liquid pH is 8, carries out the amidoxim of nano fibrous membrane.The reaction temperature of amidoxim is 110 DEG C;During amidoximation Concentration 35wt.% of oxammonium hydrochloride.;The amidoxim time is 50min;Described oxammonium hydrochloride. input amount and PAN nanofiber membrane The mol ratio of middle itrile group (-CN) is 1:0.1.Hydroxylamine hydrochloride solution regulates by adding ammonia, and the quality of described ammonia is divided Number is 10%.
Activation: oximate immerses in acid solution after terminating can obtain sea water bittern nano fibrous membrane after activation processing;Sea Water salt nano fibrous membrane is 240min in the time that acid solution processes.
Filter: with the sea water bittern nano fibrous membrane obtained, salt is filtered, obtain exquisite saturated bittern.
Prepared by step 2, Herba suadeae glaucae salt extracting solution
(1) extraction:
A, by fresh Herba suadeae glaucae, naturally dry, dry rear moisture content 2%, pulverized by pulverizer, be ground into 20 mesh, by pulverize after Herba suadeae glaucae is put in hanging basket.
B, hanging basket is put into ultrasound wave and microwave cooperating strengthening outer circulating extracting tank, and throw in the most exhausted Dry Herba suadeae glaucae and ethanol water solid-to-liquid ratio are 1:2, and the percent by volume wherein containing ethanol in ethanol water is 20%.
In C, ultrasound wave and microwave cooperating strengthening outer circulating extracting tank, material is 120MHz in frequency, the microwave of power 3KW Being 30kHz with frequency, power is the ultrasonic synergistic strengthening outer circulating extracting of 2KW, and Extracting temperature is 30 DEG C, and extraction time is 50 Minute, it is thus achieved that extracting solution inject high-order extracting solution storage tank, then strengthen outer circulating extracting tank to ultrasound wave and microwave cooperating and lead to Enter compressed air, the extracting solution remained is blown to low level extracting solution storage tank, then high position extracting solution storage tank and low level are carried in Herba suadeae glaucae Taking the extracting solution in liquid storage tank to inject in microwave decompression outer circulation concentration tank, described compressed air pressure is 0.6MPa, when being passed through Between be 20 minutes, obtain Herba suadeae glaucae salt liquid.
(2) enzymolysis
Herba suadeae glaucae salt liquid step C obtained adds water, in Herba suadeae glaucae powder oven dry weight: water volume ratio is the ratio of 1:2, Being positioned in container, stir at 40 DEG C, by 0.3% addition compound enzyme of Herba suadeae glaucae weight, compound enzyme contains bacillus subtilis egg White enzyme, bromelain and papain, weight proportion is 3:4:1, enzymolysis 30 minutes, and described extraction hydrolysis temperature is 30 DEG C, centrifugation after completing, collect supernatant, obtain Herba suadeae glaucae salt extracting solution.
Step 3, evaporative crystallization
By the refined saturated bittern of preparation, it is heated to 80 DEG C, makes salt be cooled to 30 DEG C with 2 DEG C/min, add the Herba suadeae glaucae of preparation Plant salt extracting solution and commercially available Folium Isatidis extract, Herba suadeae glaucae salt extracting solution addition is the 1 of saturated nacl aqueous solution volume Times, the addition of described Folium Isatidis extract is in salt the 24% of sodium chloride quality, then stirs mixing;Mixed solution is made to drop Temperature is to 10 DEG C;Introducing in the water tank with spray equipment, mixed solution is sprayed from top to bottom by spray equipment, and spray rate is 2m/h, while spray, starts blower fan, makes the wind waved spray streamline of 75 DEG C, and wind speed is 5.8m/s, and spray falls in tank Solution, squeezed in water tank by circulating pump, the most repeatedly, until air-dry crystallization.
Step 4, be dried
Salt slurry after crystallization being sent into vibrations drying bed be dried, controlling baking temperature is 70 DEG C, and dried purified salt enters Packet assembler.
By above method prepare containing sea salt and the plant salt of Folium Isatidis extract, composition includes: this product colour is light Brown, particle diameter 3mm, NaCl content: 72%, moisture: 12%, MgCl2Content: 0.01%, CaSO4Content: 0.02%, isatin Alkane B content: 12%, cupreol content: 0.3%, palmitic acid content: 0.6%,
After testing, in the plant salt containing sea salt and Folium Isatidis extract of preparation, molybdenum ion content is at 0.02mg/kg, silver ion Content 0.03mg/kg, cobalt ion content 0.03mg/kg.
Screening healthy mice 8, is divided into A, B two groups, and after two groups of white mice cuttings, leg fur wound 3mm is deep, and A group is little White mouse food adds the plant salt that the present invention produces, as A group white mice salinity main source.B group white mice food adds Adding the common table salt main source as B group white mice salinity, each salinity addition of A, B two groups keeps consistent, every day feeding 3 Secondary, continuous feeding white mice three days, in A group white mice, three wound healings, a slightly swelling, wound healing rate is 75%, B Group white mice, with congestion, heals two days later.
Use the present invention prepare containing sea salt and the plant salt of Folium Isatidis extract, place 2 years, have no caking.
Embodiment 2: containing sea salt and the preparation of the plant salt of Folium Isatidis extract
Step 1, exquisite making from brine are standby
(1) brine collection
Potassium ferrocyanide is added in the saturated bittern that pH value is 8, is prepared as the potassium ferrocyanide solution that concentration is 0.5mg/L, Add sodium carbonate and calcium chloride, stand, precipitate, filter, remove most Ca2+, Mg2+, Fe2+ plasma in salt, To the purest salt.In salt, molybdenum ion content is at 15mg/L, silver ion content 15mg/L, cobalt ion content after testing 20mg/L。
(2) filter
Mechanical filter: the salt gathered is removed bulky grain solid impurity therein and mechanicalness impurity through mechanical filter;The One layer is that activated alumina is as filtrate, the specification of filter material of described first time filtrate as filtrate, second layer selection quartz sand 4mm, specification 5mm of second layer filtrate, filter type is for filter up and down, and after double medium filtration, the turbidity of salt is less than 5NTU;
Filter-cloth filtering: again by microfiltration cloth filter plate water outlet after mechanical filter, microfiltration cloth filter plate surface covers microfiltration cloth, and its material is Filter felt or filter cotton, filtering accuracy 35 μm;It filters filtering velocity and controls at 8m/h, and filter pressure is 0.7mpa.
Nanofiltration: the salt after filtering carries out nanofiltration process, and nanofiltration temperature to control at 35 DEG C, adds reducing agent, uses Reducing agent be sodium sulfite.The addition of reducing agent is the 25% of NF membrane quality.Reducing agent is configured to the solution of 3%, nanofiltration Film precision controlling is in 7 μm, and the material of NF membrane is SPSF composite.
(3) nano fibrous membrane removing heavy metals
After filtering, clean salt, is filtered by sea water bittern nano fibrous membrane, removes heavy metal ion.Nano fibrous membrane The number of plies be 4 layers, filter pressure control 0.3MPa.The manufacture method of described nano fibrous membrane is:
Prepared by PAN spinning liquid: dimethyl fumarate and 2-methyl-2 pyrrolidone solution are mixed, dissolved by PAN, solution temperature 60 DEG C, adding ammonia after cooling, the concentration of ammonia is 20%, and the addition of ammonia and 2-methyl-2 ketopyrrolidine volume ratio are 3: 1, mix 3h, temperature controls 13 DEG C, is made into spinning solution;Dimethyl fumarate concentration is 22wt.%, 2-methyl-2 ketopyrrolidine Concentration is 25wt.%.
Spinning: by electrostatic spinning process, PAN nano wire is deposited on polyethylene terephthalate non-woven fabrics, obtain It is able to the nano fibrous membrane that polyethylene terephthalate non-woven fabrics is substrate;Spinning voltage is 17kV, relative humidity 40%; Spinning nozzle is flat type hole, and spinneret orifice cross-sectional aspect ratio is 5:1;The thickness of non-woven fabrics is 1100 μm;The thickness of PAN nano wire Being 500 μm, PAN nano wire mass content in nano fibrous membrane is 15%.
Amidoxim: PAN nanofiber membrane be immersed in the alkaline solution containing oxammonium hydrochloride., controls hydroxylamine hydrochloride solution pH It is 10, carries out the amidoxim of nano fibrous membrane.The reaction temperature of amidoxim is 125 DEG C;During amidoximation The concentration range of oxammonium hydrochloride. is at 40wt.%;The amidoxim time is 80min;Described oxammonium hydrochloride. input amount and PAN Nanowire In dimension film, the mol ratio of itrile group (-CN) is 1:0.3.Hydroxylamine hydrochloride solution regulates by adding ammonia, the matter of described ammonia Amount mark is 12%.
Activation: oximate immerses in acid solution after terminating can obtain sea water bittern nano fibrous membrane after activation processing;Sea Water salt nano fibrous membrane is 320min in the time that acid solution processes;
Filter: the sea water bittern nano fibrous membrane that will obtain, filter to obtain exquisite saturated bittern;
Prepared by step 2, Herba suadeae glaucae salt extracting solution
(1) extraction:
A, by fresh Herba suadeae glaucae, naturally dry, dry rear moisture content 4%, pulverized by pulverizer, be ground into 130 mesh, after pulverizing Herba suadeae glaucae put in hanging basket;
B, hanging basket is put into ultrasound wave and microwave cooperating strengthening outer circulating extracting tank, and throw in over dry alkali by weight percentage Fluffy is 1:3 with ethanol water solid-to-liquid ratio, and the percent by volume wherein containing ethanol in ethanol water is 40%.
In C, ultrasound wave and microwave cooperating strengthening outer circulating extracting tank, material is 160MHz in frequency, the microwave of power 6KW Being 40kHz with frequency, power is the ultrasonic synergistic strengthening outer circulating extracting of 13KW, and Extracting temperature is 40 DEG C, and extraction time is 70 minutes, it is thus achieved that extracting solution inject high-order extracting solution storage tank, then strengthen outer circulating extracting tank to ultrasound wave and microwave cooperating It is passed through compressed air, the extracting solution remained in Herba suadeae glaucae is blown to low level extracting solution storage tank, then by high position extracting solution storage tank and low level Extracting solution in extracting solution storage tank injects in microwave decompression outer circulation concentration tank, and described compressed air pressure is 0.8MPa, is passed through Time is 30 minutes, obtains Herba suadeae glaucae salt liquid.
(2) enzymolysis
Herba suadeae glaucae salt liquid step C obtained adds water, in Herba suadeae glaucae powder oven dry weight: water volume ratio is the ratio of 1:6, Being positioned in container, stir at 50 DEG C, by 6% addition compound enzyme of Herba suadeae glaucae weight, compound enzyme contains subtilisin Enzyme, bromelain and papain, weight proportion is 3:1:1, enzymolysis 120 minutes, and described extraction hydrolysis temperature is 40 DEG C , centrifugation after completing, collect supernatant, obtain Herba suadeae glaucae salt extracting solution.
Step 3, evaporative crystallization
By the refined saturated bittern of preparation, it is heated to 100 DEG C, makes salt be cooled to 40 DEG C with 3 DEG C/min, add the Herba suadeae glaucae of preparation Plant salt extracting solution and Folium Isatidis extract, Herba suadeae glaucae salt extracting solution addition is 2 times of saturated nacl aqueous solution volume, institute Stating the addition of Folium Isatidis extract is in salt the 27% of sodium chloride quality, stirring mixing;Mixed solution is made to be cooled to 15 DEG C; Introducing in the water tank of spray equipment, mixed solution is sprayed from top to bottom by spray equipment, and spray rate is 3m/h, spray Meanwhile, starting blower fan, make the wind waved spray streamline of 7 DEG C, wind speed is 6.2 m/s, and spray falls into the solution in tank, is circulated Pump is squeezed in water tank, the most repeatedly, until air-drying crystallization.
Step 4, be dried
Salt slurry after crystallization being sent into vibrations drying bed be dried, controlling baking temperature is 85 DEG C, and dried purified salt enters Packet assembler.
By above method prepare containing sea salt and the plant salt of Folium Isatidis extract, composition includes: this product colour is light Brown, particle diameter 4mm, NaCl content: 82%, moisture: 2%, MgCl2Content: 0.03%, CaSO4 Content: 0.08%, isatan B content: 1.3%, cupreol content: 0.3%, palmitic acid content: 0.7%, after testing, after testing, preparation containing sea salt and Folium Isatidis In the plant salt of leaf extract, molybdenum ion content is at 0.01mg/kg, silver ion content 0.02mg/kg, cobalt ion content 0.03mg/kg。
The healthy small test white rabbit 8 of screening, is divided into A, B two groups, leg fur wound 5mm after two groups of test white rabbit cuttings Deeply, 2cm length, A group small test white rabbit food adds the plant salt that the present invention produces, mainly comes as A group test white rabbit salinity Source.B group test white rabbit food adds the common table salt main source as B group test white rabbit salinity, two groups of each salinities of A, B Addition keeps consistent, every day feeding 3 times, continuous feeding test white rabbit three days, in A group test white rabbit, four test white rabbits hinder Completely, wound healing rate reaches 100%, and B group test white rabbit wound, with congestion, heals after three days in mouth healing.
Use the present invention prepare containing sea salt and the plant salt of Folium Isatidis extract, place 2.5 years, have no caking.
Embodiment 3: containing sea salt and the preparation of the plant salt of Folium Isatidis extract
Step 1, exquisite making from brine are standby
(1) brine collection
Potassium ferrocyanide is added in the smart saturated bittern that pH value is 9, be prepared as the potassium ferrocyanide that concentration is 0.8 mg/litre Solution, adds sodium carbonate and calcium chloride, stands, precipitates, filters, remove in salt most Ca2+, Mg2+, Fe2+ etc. from Son, obtains the purest salt.In salt, molybdenum ion content is at 20mg/L, silver ion content 20mg/L, cobalt ion after testing Content 25mg/L.
(2) filter
Mechanical filter: the salt gathered is removed bulky grain solid impurity therein and mechanicalness impurity through mechanical filter;Machine Tool filters, be for the first time activated alumina as filtrate, second layer selection quartz sand is as filtrate, the filter of described first time filtrate Gauge lattice are 5mm, specification 5mm of second layer filtrate, and filter type is for filter up and down, and after double medium filtration, the turbidity of salt is little In 5NTU;
Filter-cloth filtering: again by microfiltration cloth filter plate water outlet after mechanical filter, microfiltration cloth filter plate surface covers microfiltration cloth, and its material is Filter cotton, filtering accuracy 45 μm;It filters filtering velocity and controls at 9m/h, and filter pressure is 0.9MPa.
Nanofiltration: the salt after filtering carries out nanofiltration process, and nanofiltration temperature to control at 40 DEG C, adds reducing agent, uses Reducing agent be pyrosulfite.The addition of reducing agent is the 35% of NF membrane quality.Reducing agent is configured to the solution of 4%, receives Filter membrane precision controlling is in 68 μm, and the material of NF membrane is acetic acid-Triafol T.
(3) removing heavy metals
Clean salt after filtering, is filtered by sea water bittern nano fibrous membrane, removes heavy metal ion.Nanofiber The number of plies of film is 5 layers, and filter pressure controls 0.5mpa.The manufacture method of described nano fibrous membrane is:
Prepared by PAN spinning liquid: dimethyl fumarate and 2-methyl-2 pyrrolidone solution are mixed, dissolved by PAN, solution temperature 70 DEG C, adding ammonia after cooling, the concentration of ammonia is 25%, the addition of ammonia and 2-methyl-2 ketopyrrolidine molal weight ratio For 5:1, mixing 4h, temperature controls 15 DEG C, is made into spinning solution;Dimethyl fumarate concentration is 25wt.%, 2-methyl-2 pyrroles Alkanone concentration is 28wt.%.
Spinning: by electrostatic spinning process, PAN nano wire is deposited on polyethylene terephthalate non-woven fabrics, obtain It is able to the nano fibrous membrane that polyethylene terephthalate non-woven fabrics is substrate;Spinning voltage is 20kV, relative humidity 40%; Spinning nozzle is flat type hole, and spinneret orifice cross-sectional aspect ratio is 4:1;The thickness of non-woven fabrics is 1200 μm;The thickness of PAN nano wire Being 500 μm, PAN nano wire mass content in nano fibrous membrane is 20%.
Amidoxim: PAN nanofiber membrane be immersed in the alkaline solution containing oxammonium hydrochloride., controls hydroxylamine hydrochloride solution pH It is 9, carries out the amidoxim of nano fibrous membrane.The reaction temperature of amidoxim is 135 DEG C;Salt during amidoximation The concentration range of acid azanol is at 40wt.%;The amidoxim time is 100min;Described oxammonium hydrochloride. input amount and PAN Nanowire In dimension film, the mol ratio of itrile group (-CN) is 1:0.4.Hydroxylamine hydrochloride solution regulates by adding ammonia, the matter of described ammonia Amount mark is 12%.
Activation: oximate immerses in acid solution after terminating can obtain sea water bittern nano fibrous membrane after activation processing;Sea Water salt nano fibrous membrane is 360min in the time that acid solution processes;
Filter: the sea water bittern nano fibrous membrane that will obtain, filter to obtain exquisite saturated bittern;
Prepared by step 2, Herba suadeae glaucae salt extracting solution
(1) extraction:
A, by fresh Herba suadeae glaucae, naturally dry, dry rear moisture content 5%, pulverized by pulverizer, be ground into 50 mesh, by pulverize after Herba suadeae glaucae is put in hanging basket;
B, hanging basket is put into ultrasound wave and microwave cooperating strengthening outer circulating extracting tank, and throw in over dry alkali by weight percentage Fluffy is 1:5 with ethanol water solid-to-liquid ratio, and the percent by volume wherein containing ethanol in ethanol water is 60%.
In C, ultrasound wave and microwave cooperating strengthening outer circulating extracting tank, material is 180MHz in frequency, the microwave of power 10KW Being 50kHz with frequency, power is the ultrasonic synergistic strengthening outer circulating extracting of 5KW, and Extracting temperature is 50 DEG C, and extraction time is 100 minutes, it is thus achieved that extracting solution inject high-order extracting solution storage tank, then strengthen outer circulating extracting tank to ultrasound wave and microwave cooperating It is passed through compressed air, the extracting solution remained in Herba suadeae glaucae is blown to low level extracting solution storage tank, then by high position extracting solution storage tank and low level Extracting solution in extracting solution storage tank injects in microwave decompression outer circulation concentration tank, and described compressed air pressure is 1MPa, when being passed through Between be 50 minutes, obtain Herba suadeae glaucae salt liquid
(2) enzymolysis
Herba suadeae glaucae salt liquid step C obtained adds water, in Herba suadeae glaucae powder oven dry weight: water volume ratio is the ratio of 1:8, Being positioned in container, stir at 65 DEG C, by 1% addition compound enzyme of Herba suadeae glaucae weight, compound enzyme contains subtilisin Enzyme, bromelain and papain, weight proportion is 4:3:1, enzymolysis 160 minutes, and described extraction hydrolysis temperature is 50 DEG C , centrifugation after completing, collect supernatant, obtain Herba suadeae glaucae salt extracting solution.
Step 3, evaporative crystallization
By the refined saturated bittern of preparation, it is heated to 120 DEG C, makes salt be cooled to 360 DEG C with 4.5 DEG C/min, add preparation Herba suadeae glaucae salt extracting solution and Folium Isatidis extract, Herba suadeae glaucae salt extracting solution addition is saturated nacl aqueous solution volume 2.5 times, the addition of described Folium Isatidis extract is in salt the 25% of sodium chloride quality, makes mixed solution be cooled to 20 DEG C;Draw Entering in the water tank of spray equipment, mixed solution is sprayed from top to bottom by spray equipment, and spray rate is 4m/h, spray same Time, starting blower fan, make the wind waved spray streamline of 80 DEG C, wind speed is 6.8 m/s, and spray falls into the solution in tank, is circulated Pump is squeezed in water tank, the most repeatedly, until air-drying crystallization.
Step 4, be dried
Salt slurry after crystallization being sent into vibrations drying bed be dried, control baking temperature and be 70-90 DEG C, dried purified salt enters Enter packet assembler.
By above method prepare containing sea salt and the plant salt of Folium Isatidis extract, color light brown, particle diameter 2mm, NaCl content: 80%, moisture: 1%, MgCl2Content: 0.02%, CaSO4 Content: 0.06%, isatan B content: 0.5%, β- Sitosterol content: 0.2%, palmitic acid content: 0.6% after testing, after testing, preparation containing sea salt and the plant of Folium Isatidis extract In salt, molybdenum ion content is at 0.01mg/kg, silver ion content 0.01mg/kg, cobalt ion content 0.02mg/kg.
Screening health test Mini-musk swine 8, is divided into A, B two groups, leg fur wound 6mm after two groups of Mini-musk swine cuttings Deeply, 3cm length, A group Mini-musk swine food adds the plant salt that the present invention produces, as A group Mini-musk swine salinity main source.B group Adding the common table salt main source as B group Mini-musk swine salinity in Mini-musk swine food, each salinity addition of A, B two groups keeps Unanimously, every day feeding 3 times, continuous feeding three days, in A group Mini-musk swine, three wound healings are complete, one with a little cicatrix, Wound healing rate 75%, B group Mini-musk swine wound is with congestion.
Use the present invention prepare containing sea salt and the plant salt of Folium Isatidis extract, place 3 years, have no caking.
Embodiment 4: single factor analysis is tested
Through substantial amounts of test, it has been found that in nano fibrous membrane preparation process, in PAN spinning liquid preparation process, add one Fixed ammonia removes heavy metal ion to nano fibrous membrane and has a certain impact, and the method using embodiment 3 below is spun at PAN Silk liquid preparation process in, only change ammonia concn, response time, reaction temperature, to preparation containing sea salt and Folium Isatidis extract Plant salt in the impact of content of beary metal, such as table 1:
Table 1: in PAN spinning liquid preparation process, changes ammonia concn, response time, reaction temperature, to preparation containing sea salt and The impact of content of beary metal in the plant salt of Folium Isatidis extract
Above-mentioned test can significantly be found out, is 20% at ammonia concn, and hybrid reaction temperature is 14 DEG C, and the response time is 3.5h Time, in the plant salt containing sea salt and Folium Isatidis extract of preparation, molybdenum ion, silver ion, cobalt ion content minimum, therefore, Embodiment 7 is the optimum embodiment of this test.
Except as otherwise noted with art technology conventional unit, the percent employed in the present invention is weight percent Number, ratio of the present invention, it is mass ratio.
Finally it is noted that the foregoing is only the preferred embodiments of the present invention, it is not limited to the present invention, Although being described in detail the present invention with reference to previous embodiment, for a person skilled in the art, it still may be used So that the technical scheme described in foregoing embodiments to be modified, or wherein portion of techniques feature is carried out equivalent. All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in the present invention's Within protection domain.

Claims (10)

1. one kind contains sea salt and the plant salt of Folium Isatidis extract, it is characterised in that: NaCl content: 75-in described plant salt 85%。
It is the most according to claim 1 a kind of containing sea salt with the plant salt of Folium Isatidis extract, it is characterised in that: described plant Isatan B content in salt: 0.5-1.5%, cupreol content: 0.1-0.5%, palmitic acid content: 0.6-0.8%, molybdenum ion content ≤ 0.03mg/kg, silver ion content≤0.04mg/kg, cobalt ion content≤0.05mg/kg.
3. one kind uses the method that nano fibrous membrane removing heavy metals ion processes prepares plant salt, it is characterised in that: include exquisiteness Salt preparation process, described exquisite salt preparation process includes nano fibrous membrane removing heavy metals step, and described nano fibrous membrane removes Heavy metal step includes PAN spinning liquid preparation process, and the number of plies of described nano fibrous membrane is 3-5 layer, and filter pressure controls 0.1- 0.5MPa。
A kind of method using nano fibrous membrane removing heavy metals ion processes to prepare plant salt the most according to claim 3, It is characterized in that: described PAN spinning liquid preparation process, spinning liquid preparation process needs add ammonia.
A kind of method using nano fibrous membrane removing heavy metals ion processes to prepare plant salt the most according to claim 4, It is characterized in that: the concentration of the ammonia of described addition is 15-25%.
A kind of side using nano fibrous membrane removing heavy metal ion technique to prepare plant salt the most according to claim 4 Method, it is characterised in that: after described addition ammonia, incorporation time is: 2-4h, and temperature controls: 10-15 DEG C.
A kind of method using nano fibrous membrane removing heavy metals ion processes to prepare plant salt the most according to claim 3, It is characterized in that: described nano fibrous membrane removing heavy metals step also includes that spinning process, described spinning process spinning nozzle are flat Type hole, spinneret orifice cross-sectional aspect ratio is 4:1.
A kind of method using nano fibrous membrane removing heavy metals ion processes to prepare plant salt the most according to claim 3, It is characterized in that: described nano fibrous membrane removing heavy metals step also includes amidoxim step;Described amidoxim step be by PAN nanofiber membrane is immersed in the alkaline solution containing oxammonium hydrochloride. process, and the reaction temperature of described amidoxim is 110- 145℃。
A kind of method using nano fibrous membrane removing heavy metals ion processes to prepare plant salt the most according to claim 8, It is characterized in that: the pH value of described hydroxylamine hydrochloride solution is 8-11.
A kind of method using nano fibrous membrane removing heavy metals ion processes to prepare plant salt the most according to claim 9, It is characterized in that: use ammonia regulation hydroxylamine hydrochloride solution pH value.
CN201610282891.3A 2016-05-03 2016-05-03 Sea salt and folium isatidis extract containing plant salt and method for preparing plant salt by using heavy metal ion removal process through nanofiber membrane Withdrawn CN105942431A (en)

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