CN103931644B - Bactericidal and preservative agent combination for repair-regeneration of microbial pollution products - Google Patents
Bactericidal and preservative agent combination for repair-regeneration of microbial pollution products Download PDFInfo
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Abstract
The invention relates to a bactericidal and preservative agent combination for the repair-regeneration of microbial pollution products, which comprises the following active ingredients: a preservative agent A, a preservative agent B, a bactericide, solvents, additives and water, wherein the preservative agent A is formed by bronopol, the preservative agent B is formed by parachlorometaxylenol PCMX and a phenoxyethanol mixture, and the bactericide is formed by 2,2-dibromo-3-nitrilo-propionamide DBNPA or polyhexamethylene biguanidine hydrochloride PHMB. Through one-time addition, the bactericidal and preservative agent combination disclosed by the invention has strong synergistic, preservative and bactericidal effects, and can concurrently have the functions of bactericidal repair and corrosion and mildew prevention in the period of re-storage, thus most of industrial water-based products metamorphosed by microbial pollution are reused. The bactericidal and preservative agent combination disclosed by the invention has the advantages of reasonable formula, advanced process, high cost performance, low toxicity, good operational feasibility, bactericidal and preservative effect, and the like, and is verified through a lot of industrial practices.
Description
Technical field
The invention belongs to the preparing technical field of chemical sterilization preservative, relate to a kind of reparative regeneration sterilization antiseptic composition of microbial contamination product, particularly a kind ofly use required efficient sterilizing antiseptic composition again for the commercial waterborne product reparation after going bad by microbial contamination.
Background technology
Aqueous industrial product such as the products such as various washing agent, daily use chemicals auxiliary agent, paper making additive, water treatment agent, coating, adhesive, metal working fluid contain the organic matter such as moisture and multiple additives due to interior, for microbial growth, breeding provide abundant carbon source, nitrogenous source, mineral salt and growth factor, very easily contamination and deterioration, and every year because commercial waterborne product is very huge by the go bad economic loss brought of microbial contamination, and therefore related go out problem of environmental pollution.Only water paint one estimation, deterioration rate (actual conditions have exceeded this value) costing bio disturbance according to average annual 3%, the whole nation loss about 400,000,000 yuan of a year.And can also see everywhere in production scene, few to hundreds of on kilogram, how arbitrarily discarded by after microbial contamination to the water paint product of tens tons, while economic loss, caused again serious environmental pollution.Except water paint, other commercial waterborne product contaminated rotten after the economic loss brought equally also very seriously and be difficult to again estimate.
People treated the method for disposal of rotten water-based industrial products and are in the past: (1), directly pour environment into disposal of refuse; (2) conventional preservatives short-term preservation is added after, high temperature twice-cooked stir-frying sterilizing being carried out to high-value product.Because usual industry heating sterilizing can not thorough killing microorganisms, also need the energy of at substantial, furthermore some thermal sensitivity product can not stand high-temperature sterilization, so people still adopt the mode of waste treatment more often than not.
In recent years, some producer is when processing deteriorating items, also adopt and exceed conventional usage amount ten doubly even more isothiazolinone, formaldehyde or cationic germicide process, but have little effect, can not tackle the problem at its root, and cause precipitation (in Kathon CG, a large amount of magnesium salts causes salt bunch), environmental pollution (formaldehyde), flocculation (cationic germicide and product in the effect of anion surfactant) etc.
Be most commonly used to 2 of upper 20% of water treatment biocide so far, 2-bis-bromo-3-nitrilo-propionamide (DBNPA) solution, and water treatment biocide is the earliest the DOW-7287 reverse osmosis water bactericide of U.S. Tao Si, (Chinese patent 200780049454.6) report for water treatment sterilization is combined in current this area also handlebar DBNPA and PHMB (hexamethylene), domestic is supplied the product in market in 2007 with " HR-V119 deteriorating items sterilization antiseptic " by present invention applicant the earliest for the process of microbial contamination deteriorating items, its sterilization component is exactly DBNPA.
But the DBNPA solution of single component has very large defect on Production and application, be mainly manifested in: (1), the in a solvent DBNPA of dissolving 20% or higher concentration are very difficult, need long-time stirring, also need heating winter, consumes energy makes again DBNPA active ingredient decompose loss, and viscosity is large, operation uses inconvenient; (2), that DBNPA adds deteriorating items rear stability to is poor, easy layering, variable color, and physical property recovers the state less than conventional products; (3), DBNPA solution only plays bactericidal action, and it very easily decomposes at typical condition, particularly pH value be greater than use in the deteriorating items of 7 time the half life period very little, about week age just decomposes totally, cannot between continuation storage period antiseptic and inhibiting bacteria function; (4), DBNPA solution place the cycle short, sealing lucifuge under normal temperature only have six months.
Summary of the invention
The object of the invention is to solve prior art Problems existing, there is provided a kind of and fill a prescription rationally, technique is advanced, cost performance is high, the reparative regeneration sterilization antiseptic composition of operation possibility and the effective microbial contamination product of sterilization and anticorrosion, this sterilization antiseptic composition is added by disposable, sterilization reparation and storage life anticorrosive mildewproof function again can be taken into account, make the rotten commercial waterborne product of most microbial contamination obtain regeneration again.
The active ingredient of the reparative regeneration sterilization antiseptic composition of the microbial contamination product provided for realizing foregoing invention object is made up of the raw material of substance of following weight percentage:
Preservative A 3% ~ 5%, preservative B 8% ~ 15%,
Bactericide 5% ~ 15%, solvent 60% ~ 70%,
Auxiliary agent 0.1% ~ 0.5%,
Surplus is water;
Described preservative A is bronopol (the bromo-2-nitropropane-1 of 2-, 3 glycol, that is Bronopol), described preservative B is to chloro-3,5-xylenol (PCMX) and Phenoxyethanol press the mixture of the part by weight configuration of 1:1.25 ~ 8, described bactericide is 2,2-bis-bromo-3-nitrilo-propionamide (DBNPA) or hexamethylene (PHMB), described solvent is 1,2 propane diols and/or dipropylene glycol and/or methyl propanediol, described auxiliary agent is formic acid and/or hydrochloric acid and/or sulfuric acid.
The preferred weight part ratio range making the raw material of substance of the reparative regeneration sterilization antiseptic composition of microbial contamination product of the present invention is:
Preservative A 3% ~ 4%, preservative B 10% ~ 15%,
Bactericide 9% ~ 11%, solvent 65% ~ 70%,
Auxiliary agent 0.1% ~ 0.3%,
Surplus is water.
The further technical solution of the present invention is also: described bactericide is DBNPA (DBNPA), and described solvent is methyl propanediol, and described auxiliary agent is formic acid.
The effect that in the present invention's formula, each component materials raw material is respective had in sterilization antiseptic composition is as described below.
Bronopol (Bronopol) is sterilization antiseptic very efficiently, is mainly used in the mildew-resistant of paper making pulp, coating and daily cosmetics, anticorrosion.The sterilization and anticorrosion ability utilizing its wide spectrum in the present compositions.
To chloro-3,5-xylenol (PCMX) is a kind of antimildew and antibacterial agent of safe, efficient, wide spectrum, low toxicity, to most Gram-positive, negative bacterium, fungi, mould kills effect, non-stimulated, hypotoxicity, be the first-selected germ killing drugs through U.S. FDA approval, its chemical stability is good, can not inactivation under usual storage requirement.PCMX effect is in the present compositions quick sterilization and antibacterial anticorrosion at product storage period, takes into account certain gas phase antisepsis (PCMX has certain Gas distribution) simultaneously.
Phenoxyethanol is a kind of typical antibacterial aseptic production, all inhibited to bacterium, saccharomycete and mould, also there is certain sterilizing ability simultaneously, particularly very high to the kill efficiency of pseudomonad, and pseudomonad is general a large amount of existence in deteriorating items.Phenoxyethanol another effect is in the present compositions space sterilization, can make full use of the bactericidal potency of its volatile quantity gas.
DBNPA (DBNPA) has the bactericidal property of wide spectrum, to bacterium, fungi, saccharomycete, algae, biological clay and threaten the pathogenic microbes etc. of human health all to have good killing effect.DBNPA feature is that sterilization speed is exceedingly fast, and efficiency is high, and within 5 ~ 10 minutes, sterilizing rate can reach more than 99%, degrades rapidly after killing microorganism.Only have and kill most microorganism fast, that could suppress polluted product continues rotten deterioration.Therefore the product peculiar smell that DBNPA effect is in the present compositions quick sterilization and eliminates because contamination and deterioration brings.
Hexamethylene (PHMB) is a kind of quick fungicide with cationic characteristic, and toxicity is extremely low, can use in the system existed without anion surfactant.
Methyl propanediol and/or 1,2 propane diols and/or dipropylene glycol are transparent low-viscosity (mobile) liquid, and when room temperature is liquid, particularly methyl propanediol is almost non-toxic for above-mentioned solvent, to skin and eye irritation, is ratified by FDA.Main Function is in the present compositions the dissolubility and relative low viscosity that utilize it good.
Formic acid and/or hydrochloric acid and/or sulfuric acid are as auxiliary agent, and one is the necessary pH value of adjustment stable system, the space sterilization and anticorrosion ability simultaneously utilizing it certain.
By above-mentioned each raw material of substance with the use of, serve the effect of " learn from other's strong points to offset one's weaknesses, bring out the best in each other ", the result of compound, raising drug effect while also can reduce addition, particularly as the present invention by the preservative of several different mechanism of action with the use of time Be very effective.
Method for the preparation of this reparative regeneration sterilization antiseptic composition comprises following processing step:
1, obtain the solution of preservative A after being dissolved in water by bronopol, used additives adjusted to ph is to 3.5 ~ 4;
2, by preservative B, bactericide and the stirring solvent dissolving accounting for solvent composition gravimetric value 30% ~ 40%, the solution of anticorrosion and bactericidal agent is obtained;
The solution of the preservative A 3, step 1 obtained under agitation adds in the solution of the anticorrosion and bactericidal agent of step 2 gained and stirs;
4, add remaining solvent to stir evenly, used additives adjusted to ph, to 3.5 ~ 4, obtains reparative regeneration sterilization antiseptic composition product.
The preparation method of a kind of optimization of the present invention comprises following processing step:
1, preservative solution A is obtained after being dissolved in water by bronopol, by formic acid adjusted to ph to 3.5 ~ 4;
2, will to chloro-3,5-xylenol and Phenoxyethanol (preservative B), 2,2-bis-bromo-3-nitrilo-propionamide or hexamethylene (bactericide) and account for the methyl propanediol stirring and dissolving of solvent composition gravimetric value 30% ~ 40%, obtain the solution of anticorrosion and bactericidal agent;
The solution of the preservative A 3, step 1 obtained under agitation adds in the solution of the anticorrosion and bactericidal agent of step 2 gained and stirs;
4, add remaining methyl propanediol to stir evenly, by formic acid adjusted to ph to 3.5 ~ 4, obtain reparative regeneration sterilization antiseptic composition product
The beneficial effect that the present invention has is as described below.
One, the careful property of technical scheme of the present invention is strong.Because the resistance of microorganism constantly strengthens, often kind of preservative has oneself specific fungicidal spectrum, is all-round without any a kind of preservative, the key point of this problem of easy microbial contamination of certain sterilization antiseptic of single use often.Be used alone the DBNPA of 20% in the past in deteriorating items, and only had bactericidal action, and relative quantity is large, easily makes product physical property change, and can not play the antiseptic and inhibiting bacteria function effect continued when storing.The present invention is low and have the preservative A of sterilization and anticorrosion effect and preservative B and combinationally use with it by toxicity, taken into full account complementation and chemical compatibility and the toxicological security of the building performance and bactericidal spectrum between several active principle, formed have can quick sterilization again can a kind of reparative regeneration sterilization antiseptic composition of the industrial products that go bad by microbial contamination of anticorrosive mildewproof.
Two, containing quick sterilization composition in the reparative regeneration sterilization antiseptic composition of microbial contamination product of the present invention, antibacterial anticorrosive mildewproof composition and space antisepsis and sterilization composition in system, expand use effect, it not only can be used for the reparation reuse of contamination and deterioration commercial waterborne product, and at water treatment sterilization algae removal production system (equipment, pipeline cleaning sterilization) in also have beat all good effect, also be used in ore pulp simultaneously, sewage treatment equipment, art fountain, reverse osmosis and ultrafiltration system, evaporative condenser, the paper pulp used in the equipment systems such as heat exchanger cycle water system and paper treat liquid and additive, starch, emulsion, dispersion liquid, latex, coating, adhesive, putty and sealant, carpet back-adhesive and laminating adhesive, industrial bonding agent, metal working fluid, conveyer lubricant, hydraulic fluid, leather and leather and fur products, the Antisepticize and mildew preventive of the aqueous products such as textile auxiliary.
Three, the toxicity of sterilization antiseptic composition of the present invention is low, and safety is high, once adds separately and can effectively repair by the rotten product of microbial contamination, and at storage life anticorrosive mildewproof again.DBNPA and the special decolouring and deodorizing effect of related component in said composition, the variable color that most polluted product can be made to cause because of microbial action and peculiar smell can recover normal condition; Product after process can supplement a small amount of main component be decomposed by the microorganisms if desired, and adjusts the normal value of pH value to product.
Four, the good stability of the reparative regeneration sterilization antiseptic composition of microbial contamination product of the present invention, the normal temperature storage phase is greater than 12 months.
Five, the present invention adopts composite bactericidal anticorrosive mildewproof component, and effect is very remarkable, usually just can reach the object of repairing and preserving when addition is 0.2% ~ 0.8% according to contamination of products degree.
Six, the production operation of the reparative regeneration sterilization antiseptic composition of microbial contamination product of the present invention is simple, is easy to realize large-scale production.
Embodiment
The present invention will be further described by the following examples.It is noted that to one skilled in the art, do not depart from principle of the invention framework basis on can make some modification, but these all should be considered as belonging to protection scope of the present invention.
Embodiment
The reparative regeneration of the microbial contamination product preparation example of sterilization antiseptic composition
According to the aforesaid preparation process of the present invention, the reparative regeneration sterilization antiseptic composition of microbial contamination product is prepared by each raw material components provided in table 1, the formulation samples of five groups of sterilization antiseptic compositions of 1-5 is numbered in obtained table 1, each component all by weight, and all amounts to into pure material metering.
Table 1: the composition (%) of the several formula of the present invention
The good stability of the reparative regeneration sterilization antiseptic composition of microbial contamination product of the present invention, product normal temperature storage carried out efficient liquid phase chromatographic analysis after 13 months, and various active ingredient change is very little, and stability has large lifting (table 2).In table, change in concentration is analytical error for "+".
Table 2: sterilization antiseptic composition of the present invention compares with the stability of the DBNPA of 20%
Minimum inhibitory concentration (MIC) value weighs a kind of important indicator of sterilization antiseptic efficiency.Under normal circumstances, minimum inhibitory concentration (MIC) value is less, and its sterilization and anticorrosion efficiency is higher.By spread plate and dilution cultivation, minimum inhibitory concentration (MIC) value to common microbiological when testing composition of the present invention and be used alone DBNPA, the results are shown in table 3.
Table 3: MIC value (active matter is all converted into 20%) (mg/kg) of prescription of the present invention and single bactericide DBNPA
The microbiological test of table 3 has comprised single culture and mixed bacteria (mixed microorganism is the mixture of each microorganism in above-mentioned table 3), no matter be to which kind of microorganism, obvious synergistic effect is had after compound, its bactericidal effect is all better than the result being used alone DBNPA, particularly No. 5 sample proportioning most pronounced effects, No. 3 and No. 4 samples also very outstanding.But No. 5 sample combination contain the PHMB in a large number with cationic property, and purposes is subject to a lot of limitation, can only be used for not containing the system of anion surfactant.So No. 3 and No. 4 samples have more representativeness.
The practical application effect of the reparative regeneration sterilization antiseptic composition of microbial contamination product of the present invention is very good, through hundreds of practical applications inspection, has reduced economic loss, avoids environmental pollution.Below with rotten coating and chain lubricant and wipe car wet tissue for representative its outstanding sterilization regeneration effect is described.
In August, 2012, within after Xi'an coating factory about 10 batches of more than 20 ton paint fillings 5 days, find that color and luster is rubescent, then frowziness after 10 days.Its microorganism detection result is as table 4.
Table 4: the microorganism detection result of contaminated rotten coating
| Medium | Test item | Testing result (cfu/g) |
| TSA medium | Total plate count | 5.6x10 4 |
| Sabouraud culture medium | Total plate count | 1.5x10 6 |
| Rose bengal medium | Total number of fungi | 1.5x10 5 |
Accordingly, present invention applicant uses above-mentioned No. 3 composition sample 0.5% to repair, and gets sample simultaneously and does comparative trial with the DBNPA of one-component 20%.Place 6 months in the environment, routine test total plate count, result is as shown in table 5.Because in rotten coating products, film forming agent reduces to some extent, after suitably supplementing, result of use is unaffected.Result shows: reparation sterilization antiseptic composition of the present invention uses in rotten coating, recovers to maintain the original color and luster of coating, and deposits 6 months still maintenance coating not microbial contaminations, and effect is ideal.Reparation coating then only can be made to keep 30 days with the single bactericide DBNPA of identical amount, just there is serious point water in outward appearance, color and luster turns yellow, and rotten variable color, occurs peculiar smell, illustrate that DBNPA can only do bactericide use, be difficult to reach anticorrosive mildewproof effect subsequently.
Table 5: the present invention is used for the effect of rotten coating
Composition of the present invention is also used for the industrial chain lubricant having peculiar smell, color and luster burnt hair by applicant.Containing the potassium oleate of 12% in the composition of this chain lubricant, the non-ionic surface active agent of 4% and a small amount of auxiliary agent.Content of microorganisms after pollution is as table 6.Through No. 4 composition sample process of 0.4%, 24 hours outward appearances and smell recover normal, and continue to come into operation as normal product, result of use does not change.Sample after treatment deposits 1 year again, and all are normal, and microorganism testing situation is as table 6.
Table 6: the present invention is used for the effect of rotten chain lubricant
In addition, composition of the present invention is also used for the process (pollution wet tissue mainly contains bacterium and causes, and clump count is 1.1x105) occurring the wiping car wet tissue of peculiar smell by microbial contamination by applicant.By two kinds of processing methods, first be by pollute wet tissue in boiling water, boil sterilization in 20 minutes after add 0.2% isothiazolinone; Second method adds aforesaid No. 5 reparations directly to pollution wiping car wet tissue to use sterilization antiseptic composition sample 0.2% again.Observation test outward appearance and content of microorganisms (table 7) after half a year, heat and produce peculiar smell once again by the wiping car wet tissue of isothiazolinone process, microbial contamination is serious; And directly process by sterilization antiseptic composition sample again with aforesaid No. 5 reparations, outward appearance and microbiological indicator are all qualified.
Table 7: the present invention is used for having produced the effect that peculiar smell wipes car wet tissue
Claims (3)
1. the reparative regeneration of a microbial contamination product sterilization antiseptic composition, is characterized in that said composition is made up of the raw material of substance of following weight percentage:
Preservative A 3% ~ 5%, preservative B 8% ~ 15%,
Bactericide 5% ~ 15%, solvent 60% ~ 70%,
Auxiliary agent 0.1% ~ 0.5%,
Surplus is water;
Described preservative A is bronopol, described preservative B is to chloro-3,5-xylenol and Phenoxyethanol press the mixture of the part by weight configuration of 1:1.25 ~ 8, described bactericide is 2,2-bis-bromo-3-nitrilo-propionamide, described solvent is methyl propanediol, and described auxiliary agent is formic acid.
2. the reparative regeneration sterilization antiseptic composition of microbial contamination product according to claim 1, is characterized in that said composition is made up of the raw material of substance of following weight percentage:
Preservative A 3% ~ 4%, preservative B 10% ~ 15%,
Bactericide 9% ~ 11%, solvent 65% ~ 70%,
Auxiliary agent 0.1% ~ 0.3%,
Surplus is water.
3., for the preparation of a reparative regeneration method for sterilization antiseptic composition for microbial contamination product described in claim 1 or 2, it is characterized in that comprising following processing step:
3.1 bronopol is dissolved in water after obtain the solution of preservative A, used additives adjusted to ph is to 3.5 ~ 4;
3.2, by chloro-MX and Phenoxyethanol, DBNPA and the methyl propanediol stirring and dissolving accounting for solvent composition gravimetric value 30% ~ 40%, obtain the solution of anticorrosion and bactericidal agent;
The solution of 3.3 preservative A step 3.1 obtained under agitation adds in the solution of the anticorrosion and bactericidal agent of step 3.2 gained and stirs;
3.4 add remaining methyl propanediol stirs evenly, and by formic acid adjusted to ph to 3.5 ~ 4, obtains reparative regeneration sterilization antiseptic composition product.
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| CN105887562A (en) * | 2016-06-09 | 2016-08-24 | 南京晶云化工有限公司 | Papermaking antibacterial preservative and preparation method thereof |
| CN106035360A (en) * | 2016-06-20 | 2016-10-26 | 河南中天恒信生物化学科技有限公司 | Novel composite herbicide and application thereof |
| SG11202102429SA (en) * | 2018-10-04 | 2021-04-29 | Celanese Int Corp | Process for producing aqueous coating compositions |
| CN110257033B (en) * | 2019-06-04 | 2021-09-10 | 中国海洋石油集团有限公司 | Water-based cleaning solution and preparation method and application thereof |
| CN110710530B (en) * | 2019-10-09 | 2021-09-21 | 广州海源生物科技有限公司 | Compound disinfectant composition and disinfection method |
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Address after: No.61 Xiyan Road, Yanta District, Xi'an City, Shaanxi Province, 710054 Patentee after: Shaanxi Chemical Research Institute Co.,Ltd. Address before: No.61 Xiyan Road, Xi'an City, Shaanxi Province 710054 Patentee before: SHAANXI RESEARCH DESIGN INSTITUTE OF PETROLEUM CHEMICAL INDUSTRY |