CN106689126A - Polyhexamethylene guanidine effervescent preparation and preparing method thereof - Google Patents
Polyhexamethylene guanidine effervescent preparation and preparing method thereof Download PDFInfo
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- CN106689126A CN106689126A CN201611159041.0A CN201611159041A CN106689126A CN 106689126 A CN106689126 A CN 106689126A CN 201611159041 A CN201611159041 A CN 201611159041A CN 106689126 A CN106689126 A CN 106689126A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
- A01N47/42—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
- A01N47/44—Guanidine; Derivatives thereof
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Abstract
The invention relates to a polyhexamethylene guanidine effervescent preparation and a preparing method thereof. The polyhexamethylene guanidine effervescent preparation is prepared from, by mass, 1-50% of polyhexamethylene guanidine salt, 1-5% of wetting agent, 10-30% of acid agent, 20-40% of alkaline agent, 2-6% of wrapping agent, 0-8% of lubricating agent and 0-30% of filling agent, wherein fatty alcohol-polyoxyethylene ether serves as the wetting agent. The polyhexamethylene guanidine effervescent preparation has the advantages of good bactericidal and antibacterial performance, good stability, high dispersion speed, small dispersion liquid surface tension and the like, and is suitable for the fields of industry, agriculture, medicine, daily life and the like.
Description
Technical field
The present invention relates to disinfectant technical field, and in particular to a kind of polyhexamethylene guanide effervescent formulation and its preparation side
Method.
Background technology
With gradually stepping up for people's quality of the life, healthy and safe sterile products and composite antibacterial suppression becteriums product are therewith
It is fast-developing.The following several classes of disinfectant point：Phenols, alcohols, aldehydes, chlorine-containing disinfectant, quaternary ammonium salt, iodine etc..Polyhexamethylene guanide
It is a kind of environment-friendly type macromolecule polymer bactericide, it has broad-spectrum, long-term antibacterial, work fast and has no side effect
Advantage, polyhexamethylene guanide is colourless, odorless, nontoxic, non-ignitable, not quick-fried, corrosion-free, stable in properties, soluble in water, uses safety etc.
Premium properties makes it have extremely extensive purposes in industrial, agriculture, medical and daily life.The sterilization of polyhexamethylene guanide
Principle is：Guanidine active cation group combines all kinds of bacteriums, virus (negatively charged), and the splitting function of anti-microbial virus makes
Bacterial virus loses fecundity；Polyhexamethylene guanide polymeric membrane blocks the respiration channel of microorganism, microorganism is stopped up rapidly
Breath and it is dead.The antibacterial principle of polyhexamethylene guanide is：Acted on by solubilizing lipids, change the permeability of bacterial cell membrane, make bacterium
There is obstacle and there is long-acting bacteriostatic to act in internal metabolism.
Tablet, granular pattern disinfectant products have valid density high, are welcome by people the advantages of easy to carry, but piece
There is problems of dissolution in agent, granular pattern disinfectant products, its active ingredient dissolves, spreads in the solution, dispersed ground process compared with
For slow.Effervescent tablet, the design of effervescence granular formulation solve the problems, such as active ingredient rapid dispersion, but high concentration is poly- six sub-
Methylguanidine is due to its very strong hygroscopicity and larger surface tension effects (0.1% 25 DEG C of polyhexamethylene guanide aqueous solution surface
Tension force 58dyn/cm2) so that the active ingredient of polyhexamethylene guanide is in tablets in the presence of very strong sticking effect so as to influence pressure
The continuous operation of piece and the long-time stability of tablet and powder.In addition, the larger surface tension of polyhexamethylene guanide causes its effective
Disperse slow at low pole, the nonpolar interface that is sterilized after composition effervesce, and wetting action is weaker during due to bactericidal
Suction-operated of the polyhexamethylene guanide in bacterium, viral micro-organisms is had a strong impact on, weakens its bactericidal ability.
Therefore, develop the good polyhexamethylene guanide effervescent formulation of a kind of dispersive property, stability, tablet forming technique turn into work as
Preceding industry in the urgent need to.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of polyhexamethylene guanide effervescent formulation, this hair
The polyhexamethylene guanide effervescent formulation active constituent content of bright offer is high, dispersion liquid surface tension is small, with bactericidal performance
Well, the advantages of disperseing quick, it is adaptable to the field such as industrial, agriculture, medical and daily life.
Preparation method another object of the present invention is to provide above-mentioned polyhexamethylene guanide effervescent formulation.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of polyhexamethylene guanide effervescent formulation, the polyhexamethylene guanide effervescent formulation is by mass percentage by with the following group
It is grouped into：
Wherein, the wetting agent is AEO.
Inventor has found when attempting preparing a kind of polyhexamethylene guanide effervescent formulation, if polyhexamethylene guanide is prepared into
Effervescent formulation through effervesce dispersion rear solution surface tension it is larger, laboratory proofing work as polyhexamethylene guanide concentration of aqueous solution
For 0.02% when, the surface tension of the aqueous solution is 58dyn/cm2, this causes the active ingredient of polyhexamethylene guanide effervescent formulation to exist
Cannot effectively be infiltrated after effervesce, soaked, penetrated into and be sterilized interface, during due to bactericidal wetting action it is weaker have a strong impact on it is poly-
Suction-operated of the hexa-methylene guanidine in bacterium, viral micro-organisms, and then weaken its bactericidal ability.
To reduce the surface tension of the polyhexamethylene guanide effervescent formulation aqueous solution, inventor has done numerous trials, through repeatedly
Experiment inventor has found that relative to polyhexamethylene guanide high molecular polymer AEO has relatively low surface
Power, good wettability, and dielectric surface can with quick humidification, sprawl.In addition, AEO is due to hydrogen
The effect of key shows as water solubility, so being adapted to be applied in effervescent product.If inventor is further it was found that, will
After AEO is compounded with polyhexamethylene guanide, both can produce synergy, significantly reduce the table of the aqueous solution
Face tension force.The present invention is compounded AEO with poly- six subunits base melon, significantly reduces effervesce rear solution
Surface tension, improve wetting, the bactericidal performance of poly- six subunits base melon active ingredient.
Preferably, the polyhexamethylene guanide effervescent formulation is composed of the following components by mass percentage：
Wherein, the wetting agent is AEO.
Preferably, the wetting agent is end capped polyether.
In the present invention, the surface tension of normal-butyl endcap fatty alcohol polyethers and polyhexamethylene guanide compounding rear solution and
Wettability is significantly better than other AEO nonionic surfactants, it is preferred that the wetting agent is
Normal-butyl endcap fatty alcohol polyethers.
It is further preferable that the cloud point of the normal-butyl endcap fatty alcohol polyethers is 25~27 DEG C.Because cloud point is herein
In the range of normal-butyl endcap fatty alcohol polyethers there is relatively low surface tension, and with preferable water-soluble and foaming properties.
In the present invention, most preferably, the trade names of the normal-butyl endcap fatty alcohol polyethers can be LT104.
In the present invention, the poly (hexamethylene) is polyhexamethylene list guanidinesalt and/or cosmocil stearate.
Preferably, the sour agent is one or more of citric acid, tartaric acid or fumaric acid；The alkaline agent is bicarbonate
One or more of sodium, saleratus, sodium carbonate, potassium carbonate.It is further preferable that the sour agent is anhydrous citric acid or rich horse
Acid, the alkaline agent is sodium acid carbonate.
Verified through lot of experiments, using polyethylene glycol as coating agent, can preferably wrap up sour agent, the sour agent of shielding, alkali
Reaction of the agent when being in close contact.From sodium carboxymethyl cellulose solution or polyvinylpyrrolidone ethanol solution as parcel
During agent, the effervescent formulation for preparing has preferable humidity resistance and shields the reaction between sour agent, alkaline agent.
It is preferred that the coating agent is polyethylene glycol, sodium carboxymethyl cellulose solution or polyvinylpyrrolidone
Ethanol solution.It is further preferable that the coating agent is Macrogol 6000, the sodium carboxymethylcellulose that mass concentration is 1~2%
The aqueous solution or PVP K30 ethanol solution.
Preferably, the filler is sodium carboxymethyl starch.
The selection of lubricant is also most important, and inventor has found after passing through repeatedly trial, when from fumaric acid, poly- second two
When alcohol or sodium chloride are as lubricant, with preferable solute effect.It is therefore preferred that the lubricant is fumaric acid, poly- second
One or more in glycol or sodium chloride.
It is further preferable that from polyethylene glycol and sodium chloride compounding as lubricant, the polyethylene glycol and sodium chloride
Mass ratio is 1:2~1：1.
In the present invention, the effervescent formulation can be effervescence granular or effervescent tablet.
The preparation method of the polyhexamethylene guanide effervescent formulation that the present invention is provided is this area conventional method, can specifically be adopted
With the following method：
S1:Sour agent, polyhexamethylene guanide are wrapped up using portion envelops agent and prepares granulates；
S2:Alkali particle is prepared using remaining coating agent parcel alkaline agent, wetting agent；
S3：Granulates, the blending of alkali particle are obtained final product into polyhexamethylene guanide effervescence granular；
S4：By the agent of polyhexamethylene guanide effervescence granular mixed lubrication, filler in S3, poly- six are obtained final product using tabletting machine
Methylene guanidine effervescent tablet.
In the present invention, polyhexamethylene guanide, wetting agent and sour agent mixing granulation or with alkaline agent mixing granulation, this hair
It is bright to be not construed as limiting.
Compared with prior art, the present invention has the advantages that：
Polyhexamethylene guanide is made effervescent formulation, and the polyhexamethylene guanide effervesce that the present invention is provided by the present invention first
Solution after preparation effervesce has relatively low surface tension between be sterilized interface, more rapidly intensive can be sterilized material various
Matter moistened surface, absorption, enhance the bactericidal efficiency of polyhexamethylene guanide effervescent formulation.
The present invention provide effervescent formulation have the advantages that effervesce quickly dissolve dispersion, effervesce material stably, it is easy to use,
The disinfectant solution for preparing is still, tasteless.The polyhexamethylene guanide effervescent formulation bactericidal property that the present invention is provided is strong, long
Effect restraining and sterilizing bacteria, odorlessness, corrosion-free, nonhazardous, preparation process is simple are adapted in industrial, agriculture, medical and daily life etc.
Field is widely popularized and uses.
Specific embodiment
The present invention is further explained with reference to specific embodiment, but specific embodiment is not to the present invention
It is limited in any way.Unless stated otherwise, it is all the present invention provide embodiments in, there is provided raw material can from market buying obtain
, primary raw material information is as follows：
Polyhexamethylene list guanidine, biguanide hydrochloride；Purchased from the Hunan clean biochemical industry of profit, content 98.2%；
Anhydrous citric acid；Purchased from Weifang Ying Xuan industry, content 99.99%；
Sodium bicarbonate；It is commercially available, content 97.8%；
PVP；Purchased from Dongying City letter Asia chemical industry, K values 27.0-32.4；
LT104；End capped polyether (C12-18+10EO of normal-butyl closing) is purchased from BASF, content 99%.
Embodiment 1
The formula such as table 1 below of the polyhexamethylene guanide effervescent formulation that embodiment 1~6 and comparative example 1~5 are provided.
The formula of the polyhexamethylene guanide effervescent formulation that the embodiment 1~6 of table 1 and comparative example 1~5 are provided
The preparation method of the polyhexamethylene guanide effervescent formulation that embodiment 1~6 and comparative example 1~3 are provided is as follows：
(1) sour agent, polyhexamethylene guanide are wrapped up using portion envelops agent and prepares granulates；
(2) alkali particle is prepared using remaining coating agent parcel alkaline agent, wetting agent；
(3) granulates, the blending of alkali particle are obtained final product into polyhexamethylene guanide effervescence granular；
(4) by the agent of polyhexamethylene guanide effervescence granular mixed lubrication, filler in (3), obtained final product using tabletting machine poly-
Hexa-methylene guanidine effervescent tablet.
With embodiment 1, difference is each component formula in comparative example 4, sour agent, alkaline agent in comparative example 4 and
Polyhexamethylene guanide is not wrapped, but is directly well mixed each component, then carries out compressing tablet using tablet agent.
The polyhexamethylene guanide disinfectant traditional for this area that comparative example 5 is provided, its preparation method is as follows：It is sub- by poly- six
Mixing obtains final product polyhexamethylene guanide disinfectant after methylguanidine adds water.
The polyhexamethylene guanide effervescent formulation that embodiment 1~6 and comparative example 1~5 are prepared is tested, test side
Method is as follows, and test result see the table below 2.
Test method
The correlated performance of the polyhexamethylene guanide effervescent formulation that various embodiments of the present invention and comparative example are provided is by such as lower section
Method is detected：
1st, surface tension detection foundation《The measure of GB/T 22237-2008 surfactant surface tension》Relevant provision
Detection method is detected.
The solution concentration that the dissolving of polyhexamethylene guanide effervescent formulation is obtained is 0.02%, and temperature of the measurement is 25 DEG C.Surface
Power is lower, represent disinfectant preferably soak at interface, adsorb, it is sterilized, antibacterial.
2nd, pH value, detects foundation《GB/T 22237-2008 surfactants》Relevant provision detection method detected.
Closer to neutrality, represent disinfectant effervesce rear solution more stimulates smaller to pH value to human body.
3rd, dissolution velocity, with a piece of or particle (0.5g) in 200ml solution, dissolved from putting into (without it is large stretch of or
Grain is terminal) statistics dissolution velocity, in terms of the second (S).
Dissolution time is shorter, represents unit product solubility property better (using Pharmacopoeia of People's Republic of China regulation 5min
Interior dissolving is entirely criterion of acceptability).
4th, effervescent product stability, product is in 40% humidity, under the conditions of 23~27 DEG C, deposits 72 hours, then detects
Rate of effervescence and effective content.
After being deposited 72 hours under specific temperature, damp condition, the rate of effervescence of effervescent formulation is shorter, and representative products are steady
Qualitative better, i.e., effervescent system is not influenceed better by ambient humidity.
5th, bacteriostasis antibiosis performance,
Bacteriostatic test, using antibacterial ring size test method in 2002 disinfection technology standard 2.1.8, the cut-back product aqueous solution is to poly-
Hexa-methylene guanidine 5~10PPM of valid density, by staphylococcus aureus (ATCC 6538), Escherichia coli (8099)
Antibacterial ring size is tested, and inhibition zone diameter is more than 7mm person, and to there is bacteriostasis, it is qualified to be judged to；Inhibition zone diameter is less than or equal to 7mm
Person, is, without bacteriostasis, to be judged to unqualified.Antibacterial (antibacterial) performance that product possesses in is judged accordingly.
6th, bactericidal property
Microbiological test is killed, using 2002 disinfection technology standard 2.1.1.7.4 Suspension quantitative bactericidal test methods, dilution
The product aqueous solution is to polyhexamethylene guanide 4500~5500PPM of valid density, 25 DEG C of temperature, action time 15min, by gold
Staphylococcus aureus (ATCC 6538), the suspension quantitative bacteric idal experiment of Escherichia coli (8099), kill logarithm value and are more than 5, sentence
For bactericidal action is qualified；Kill logarithm value and be less than 5, be judged to bactericidal action unqualified.So as to judge whether have in product use
Standby bactericidal property.
The performance test data of the embodiment 1~6 of table 2 and effervescent tablet products obtained in comparative example 1~5
Note："-" is non-effervescent formulation in upper table, in the absence of this parameter.
From the experimental data of upper table 2, the polyhexamethylene guanide effervescent tablet that various embodiments of the present invention are prepared is dissolved in
There is relatively low surface tension after water, when the aqueous solution mass concentration of effervescent formulation is 0.02% its surface tension be only 27~
29dyn/cm2, and the surface tension of liquid polyhexamethylene guanide disinfectant solution 0.02% of the prior art then up to 56~
59dyn/cm2.Relatively low surface tension can cause that the active ingredient of polyhexamethylene guanide effervescent formulation is rapidly intensive each
Plant and be sterilized material surface wetting, absorption, enhance the bactericidal efficiency of polyhexamethylene guanide effervescent formulation.Gone back by upper table 2
Understand, after stability test, the rate of effervescence and restraining and sterilizing bacteria rate of effervescent formulation are unaffected, this shows present invention preparation
Polyhexamethylene guanide effervescent formulation has preferable stability.
By contrast, any wetting agent is not added with comparative example 1, the surface tension of the effervescent formulation for preparing is too high,
The restraining and sterilizing bacteria performance and dispersive property of effervescent formulation are badly influenced.The consumption of the wetting agent in comparative example 2 is less, prepares
Although the effervescent formulation piece shape for obtaining and effervesce dissolution velocity are unaffected, the effervescent formulation effervesce that the ratio is prepared
The surface tension of the aqueous solution afterwards is higher, and then reduces absorption and bactericidal action that polyhexamethylene guanide is sterilized interface.It is right
What ratio 3 was selected is C10~C12 APGs, and because surfactant surface tension effects are poor, wettability is low, have impact on
Its antibacterial bacteriostatic, bactericidal property.With embodiment 1, difference is each component formula in comparative example 4, the acid in comparative example 4
Agent, alkaline agent and polyhexamethylene guanide be not wrapped, but directly mixed pressuring plate.Technique for packing is not selected in comparative example 4, from molten
Solution speed can be seen that and cause the long-acting stabilization of anhydrous citric acid and the uncontrollable compressed tablets shape of sodium acid carbonate without technique for packing,
The air moisture absorption, haptoreaction cause the quick consumption of the sour agent and alkaline agent in effervescent tablet, while polyhexamethylene guanide is due to having
Stronger moisture absorption ability causes the content of active ingredient to decline, and this causes the effervescent formulation not prepared from technique for packing
Less stable, drug effect cannot get guarantee steady in a long-term.Comparative example 5 is the traditional polyhexamethylene guanide disinfectant in this area,
Compared with the effervescent formulation that various embodiments of the present invention are prepared, its water diluent surface tension is larger, by aqueous solution surface for it
Tension force effect antibacterial and bacteriostasis are relatively low, carry in-convenience in use convenient, the existing defects in food_beverage industry packaging applications.
Claims (10)
1. a kind of polyhexamethylene guanide effervescent formulation, it is characterised in that the polyhexamethylene guanide effervescent formulation presses quality percentage
Than composed of the following components：
Poly (hexamethylene) 1~50%；
Wetting agent 1~5%
Sour agent 10~30%；
Alkaline agent 20~40%；
Coating agent 2~6%；
Lubricant 0~8%；
Filler 0~30%；
Wherein, the wetting agent is AEO.
2. polyhexamethylene guanide effervescent formulation according to claim 1, it is characterised in that the polyhexamethylene guanide effervesce system
Agent is composed of the following components by mass percentage：
Poly (hexamethylene) 1~40%；
Wetting agent 2~4%；
Sour agent 10~25%；
Alkaline agent 20~35%；
Coating agent 3~6%；
Lubricant 3~8%；
Filler 5~25%；
Wherein, the wetting agent is AEO.
3. polyhexamethylene guanide effervescent formulation according to claim 1 or claim 2, it is characterised in that the wetting agent is poly- for end-blocking
Ether.
4. polyhexamethylene guanide effervescent formulation according to claim 3, it is characterised in that the wetting agent is normal-butyl end-blocking
Aliphatic alcohol polyether.
5. polyhexamethylene guanide effervescent formulation according to claim 4, it is characterised in that the normal-butyl endcap fatty alcohol gathers
The cloud point of ether is 25~27 DEG C.
6. polyhexamethylene guanide effervescent formulation according to claim 5, it is characterised in that the normal-butyl endcap fatty alcohol gathers
The product designation LT104 of ether.
7. polyhexamethylene guanide effervescent formulation according to claim 1, it is characterised in that the poly (hexamethylene) is poly-
Hexa-methylene list guanidinesalt and/or cosmocil stearate.
8. polyhexamethylene guanide effervescent formulation according to claim 1, it is characterised in that the coating agent be polyethylene glycol,
Sodium carboxymethyl cellulose solution or polyvinylpyrrolidone ethanol solution.
9. polyhexamethylene guanide effervescent formulation according to claim 1, it is characterised in that the polyhexamethylene guanide effervesce system
Agent is polyhexamethylene guanide effervescence granular or effervescent tablet.
10. the preparation method of any polyhexamethylene guanide effervescent formulation of claim 1~9, it is characterised in that methods described
Comprise the following steps：
S1:Sour agent, polyhexamethylene guanide are wrapped up using portion envelops agent and prepares granulates；
S2:Alkali particle is prepared using remaining coating agent parcel alkaline agent, wetting agent；
S3：Granulates, the blending of alkali particle are obtained final product into polyhexamethylene guanide effervescence granular；
S4：By the agent of polyhexamethylene guanide effervescence granular mixed lubrication, filler in S3, poly- six methylene is obtained final product using tabletting machine
Base guanidine effervescent tablet.
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