CN104843767B - Preparation method of officinal nano-zinc oxide - Google Patents
Preparation method of officinal nano-zinc oxide Download PDFInfo
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- CN104843767B CN104843767B CN201510241797.9A CN201510241797A CN104843767B CN 104843767 B CN104843767 B CN 104843767B CN 201510241797 A CN201510241797 A CN 201510241797A CN 104843767 B CN104843767 B CN 104843767B
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Abstract
The invention provides a preparation method of officinal nano-zinc oxide. Zinc hydroxide, a surfactant and deionized water are added into a high pressure reactor according to a certain proportion; stirring is performed under certain temperature for reaction; after the reaction is ended, obtained solution is subjected to suction filtration, deionized water washing, ethyl alcohol washing and deionized water washing, and is dried under a pressure reduction condition, thus obtaining the officinal nano-zinc oxide.
Description
Technical field
The invention discloses a kind of preparation method of medicinal nano Zinc Oxide, belongs to field of medicine and chemical technology.
Background technology
Zinc Oxide is the oxide of zinc, is insoluble in water, dissolves in acid and highly basic.It is white solid, therefore also known as zinc white.
In nature, Zinc Oxide is the main component of mineral zincite.Zinc Oxide has a wide range of applications in medicine and healthcare field.Oxidation
The mixture of zinc and 0.5% ferrum oxide becomes Calamina, is the main component of medicine calamine stone.And Zinc Oxide with contain Oleum Caryophylli
The zinc oxide-eugenol dental cement that the Oleum Caryophylli of phenol is made into can be used to have a denture made and Dental Erosion.Nano level Zinc oxide particles have deodorization and
The effect of antibacterial.Zinc Oxide is also widely used in the various dermopathic article of everyday use for the treatment of and medicine.Additionally, Zinc Oxide conduct
Additive has an application in multiple material and product, including plastics, ceramics, glass, cement, lubricant, paint, ointment, binding agent,
Sealant, pigment, food（Zinc supplement agent）, battery, Ferrite Material, fire proofing and first-aid binder etc..It is a kind of use
The extremely extensive material in way.
At present, the preparation method of Zinc Oxide can be divided mainly into solid phase method, vapor phase method, liquid phase method three major types.These three methods
The nano zine oxide for meeting most purposes can be produced.
In the patent of Publication No. 103739003A, atmospheric pressure reflux method forms settled solution, profit by zinc salt and strong aqua ammonia
With the micelle of resorcinol class cup methanesulfonic acid sodium form surfactant formation as template, by the hydrophilic group of surfactant
Electrostatic attraction effect of the azochlorosulfonate acid anion to zinc ammonium complex ion carries out the fixation and enrichment of zinc ion, removes ammonia in backflow
During deposit ZnO nanoparticle and form the ZnO nano granule of dumbbell shaped.
Suliman et al. zinc chloride and sodium hydroxide are stirred at room temperature reaction 8h, and obtain zinc hydroxide one is thick
Mixed liquor, will be zinc hydroxide thick mixed liquor and polyvinylpyrrolidone and water mixed solution anti-in 160 DEG C of autoclave
8h is answered, gained ZnO solids are in 100 DEG C of dryings and then use distilled water wash.Stir during gained solid addition 300ml distilled water will be dried
High-pressure sterilizing pot heating is proceeded to after mixing washing 3h and 3h is heated at 160 DEG C, filter, use distilled water wash.Gained solid is at 450 DEG C
Under be dried 30min.
The content of the invention
Nano zine oxide is prepared in prior art is to be precipitated first to obtain zinc hydroxide then 160 by the halides of zinc
DEG C or higher temperature under react 8h time.Long period needed for prepared by gained will improve the manufacturing cost of Zinc Oxide, this
Outer to remain a small amount of chloride in the product and without reaction completely precipitant, this is using strong influence to using as medicine
The quality of the Zinc Oxide on way.The reaction in the open solution system of zinc hydroxide is prepared by zinc chloride prepares zinc hydroxide, meeting
Generate a small amount of zinc carbonate and eventually enter in product.Use during preparing nano zine oxide similar organic with PVP etc
It is too high that solvent often leads to organic solvent residual.
The present invention is added to zinc hydroxide and surfactant, deionized water in autoclave according to a certain percentage,
Stirring reaction, reacts after terminating at a certain temperature, and resulting solution is through sucking filtration, deionized water supersound washing, EtOH Sonicate
Washing, deionized water supersound washing, are dried at reduced pressure, obtain nano zine oxide.
It is provided by the present invention a kind of to prepare medicinal nano oxygen with the decomposition of zinc hydroxide in closed autoclave
The method for changing zinc, for the past method that compares, needed for the temperature of the method is low, the time of reaction is shorter, reduces the energy and disappears
Consumption, so as to reduce the cost of Zinc Oxide.The reaction in closed autoclave can effectively reduce the generation of zinc carbonate
And carry secretly in the final product.And by supersound washing in last handling process, in can effectively solve the problem that product, organic solvent is residual
The problem stayed.The Zinc Oxide produced by this method meets the standard of Chinese Pharmacopoeia, and finished product can be used as medical usage.
The present invention can be realized by below scheme：
Zinc hydroxide is added to into reaction under high pressure with surfactant, deionized water according to a certain percentage Jing after playing powder grinding
In kettle, at a certain temperature the stirring reaction regular hour, reaction terminates rear post-processing step to be included passing through resulting solution
Sucking filtration, in the case of ultrasound, be washed with deionized filtration, filter cake is filtered with washing with alcohol again, gained solid spend again from
Sub- water supersound washing, under conditions of the decompression of 0.08Mpa, 40 DEG C are dried 3h, obtain nano zine oxide；Described zinc hydroxide,
Mass percent ratio between surfactant and deionized water is：10-15%、10-30%、60-80%.
Described surfactant is fatty glyceride, fatty acid sorbitan, Polysorbate or Polyethylene Glycol hydroxyl fat
Fat acid esters.In autoclave, reaction temperature is preferably carried out between 110-150 DEG C, between response time preferred 1-3h.
Further preferably
1st, by 10g zinc hydroxide Jing beating after powder grinding, and 30g surfactants, that deionized water 60ml is added to high pressure is anti-
In answering kettle.
2nd, the stirring reaction at a temperature of 110-150 DEG C, after reaction terminates, resulting solution is gone after ultrasonic 30min
Upper liquid, gained filter cake are washed with deionized ultrasonic 30min removals upper liquid, gained solid and wash 30min with EtOH Sonicate
With nanofiltration membrane, filter cake deionized water supersound washing 30min nanofiltration membranes again.
3rd, solid obtained by upper step is dried 3h for 40 DEG C under conditions of 0.08Mpa decompressions, obtains nano zine oxide.
Especially, the ratio of mixed system is preferably：
1. zinc hydroxide：Surfactant：The mass ratio of deionized water is=1：2.5：5；
2. zinc hydroxide：Surfactant：The mass ratio of deionized water is=1：3：6；
Compared with prior art, the present invention has the advantage that：
1st, the reaction temperature for generating nano zine oxide is low, and only 110-150 DEG C, the time used is short, reduce energy consumption, so as to
Reduce production cost.
2nd, the product cut size that obtains is little, homogeneity is high, and particle size range is 3-60 nanometers, preferred 3-40 nanometers.
3rd, the purity of nano zine oxide is high, and up to more than 99.90%, content of beary metal is less than 20ppm, can be used as medicinal
Adjuvant, the production technology for supplementing the high-end pharmaceutic adjuvant nano zine oxide of China are blank.
Specific embodiment
Embodiment 1
By 10kg zinc hydroxide Jing beating after powder grinding, and 10kg fatty glycerides, that deionized water 60L is added to high pressure is anti-
In answering kettle.Stirring reaction 2h under the conditions of 110 DEG C, 20MPa, after reaction terminates, resulting solution is gone after ultrasonic 30min
Layer liquid, gained filter cake are washed with deionized ultrasonic 30min removals upper liquid, gained solid EtOH Sonicate and wash 30min use
Nanofiltration membrane, filter cake deionized water supersound washing 30min nanofiltration membranes again.Obtained by above-mentioned steps, solid exists
Under conditions of 0.08Mpa decompressions, 40 DEG C are dried 3h, obtain nano zine oxide.
The particle size range of gained nano zine oxide is 3-60 nanometers, and product purity is 99.95%.
Embodiment 2
By 15kg zinc hydroxide Jing beating after powder grinding, and 30kg fatty glycerides, that deionized water 80L is added to high pressure is anti-
In answering kettle.In 130 DEG C, 30MPa stirring reactions 2h, after reaction terminates, resulting solution go after ultrasonic 30min upper liquid,
Gained filter cake is washed with deionized ultrasonic 30min removals upper liquid, gained solid EtOH Sonicate and washs 30min NF membrane
Filter, filter cake deionized water supersound washing 30min nanofiltration membranes again.Solid obtained by above-mentioned steps reduces pressure in 0.08Mpa
Under conditions of 40 DEG C be dried 3h, obtain nano zine oxide.
The particle size range of gained nano zine oxide is 3-60 nanometers, and product purity is 99.92%.
Embodiment 3
By 10kg zinc hydroxide Jing beating after powder grinding, and 25kg fatty glycerides, that deionized water 50L is added to high pressure is anti-
In answering kettle.In 140 DEG C, 40MPa stirring reactions 2h, after reaction terminates, resulting solution go after ultrasonic 30min upper liquid,
Gained filter cake is washed with deionized ultrasonic 30min removals upper liquid, gained solid EtOH Sonicate and washs 30min NF membrane
Filter, filter cake deionized water supersound washing 30min nanofiltration membranes again.Solid obtained by above-mentioned steps reduces pressure in 0.08Mpa
Under conditions of 40 DEG C be dried 3h, obtain nano zine oxide.
The particle size range of gained nano zine oxide is 3-60 nanometers, and product purity is 99.91%.
Embodiment 4
By 10kg zinc hydroxide Jing after beating powder and grind, and 30kg Polysorbate, deionized water 60L are added to autoclave
In.In 150 DEG C, 50MPa stirring reactions 2h, after reaction terminates, resulting solution removes upper liquid, gained after ultrasonic 30min
Filter cake is washed with deionized ultrasonic 30min removals upper liquid, gained solid EtOH Sonicate and washs 30min NF membrane mistakes
Filter, filter cake deionized water supersound washing 30min nanofiltration membranes again.Solid obtained by above-mentioned steps reduces pressure in 0.08Mpa
Under the conditions of 40 DEG C be dried 3h, obtain nano zine oxide.
The particle size range of gained nano zine oxide is 3-50 nanometers, and product purity is 99.91%.
Embodiment 5
By 10kg zinc hydroxide Jing after beating powder and grind, and 30kg Polyethylene Glycol hydroxy fatty acids, deionized water 60L are added
To in autoclave.In 150 DEG C, 50MPa stirring reactions 2h, after reaction terminates, resulting solution is gone after ultrasonic 30min
Upper liquid, gained filter cake are washed with deionized ultrasonic 30min removals upper liquid, gained solid and wash 30min with EtOH Sonicate
With nanofiltration membrane, filter cake deionized water supersound washing 30min nanofiltration membranes again.Obtained by above-mentioned steps, solid exists
Under conditions of 0.08Mpa decompressions, 40 DEG C are dried 3h, obtain nano zine oxide.
The particle size range of gained nano zine oxide is 3-40 nanometers, and product purity is 99.93%.
Experimental example
Nano zine oxide prepared by embodiment 2-5 method is prepared into into suspension, ultrasonic disperse, using laser particle size point
Analyzer determines the elastic collision rate of laser and sample so as to be maintained at 5 × 104～1 × 106Secondary s- 1, then to sample grain
Footpath carries out automatically scanning, as a result as follows.
1 particle size distribution of table compares
Claims (2)
1. a kind of preparation method of medicinal nano Zinc Oxide, it is characterised in that：Zinc hydroxide is lived with surface Jing after beating powder and grind
Property agent, deionized water are added in autoclave according to a certain percentage, the stirring reaction one at a temperature of between 110-150 DEG C
The fixed time, reaction terminates rear post-processing step to be included resulting solution through sucking filtration, in the case of ultrasound, deionized water
Washing and filtering, filter cake is filtered with washing with alcohol again, gained solid deionized water supersound washing again, in the decompression of 0.08Mpa
Under the conditions of 40 DEG C be dried 3h, obtain nano zine oxide；Described zinc hydroxide, the quality between surfactant and deionized water
Percent ratio is：10-15%, 10-30%, 60-80%；
Described surfactant is fatty glyceride, fatty acid sorbitan, Polysorbate or Polyethylene Glycol hydroxy fatty acid
Ester.
2. the preparation method according to claim 1 nano zine oxide, it is characterised in that：In autoclave, the response time is 1-
Between 3h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1296916A (en) * | 2000-12-29 | 2001-05-30 | 山东大学 | Process for preparing nm powder of zinc oxide |
| CN102515246A (en) * | 2011-12-02 | 2012-06-27 | 南京林业大学 | Preparation method of porous nano zinc oxide (ZnO) |
| CN103145175A (en) * | 2013-03-14 | 2013-06-12 | 西安交通大学 | Preparation method of small-size nano-zinc oxide powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB0313432D0 (en) * | 2003-06-11 | 2003-07-16 | Ici Plc | Particulate zinc oxide |
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- 2015-05-13 CN CN201510241797.9A patent/CN104843767B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1296916A (en) * | 2000-12-29 | 2001-05-30 | 山东大学 | Process for preparing nm powder of zinc oxide |
| CN102515246A (en) * | 2011-12-02 | 2012-06-27 | 南京林业大学 | Preparation method of porous nano zinc oxide (ZnO) |
| CN103145175A (en) * | 2013-03-14 | 2013-06-12 | 西安交通大学 | Preparation method of small-size nano-zinc oxide powder |
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