CN103931627B - A kind of organic blowing agent composite synergistic fungicidal preservative - Google Patents
A kind of organic blowing agent composite synergistic fungicidal preservative Download PDFInfo
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- CN103931627B CN103931627B CN201410200746.7A CN201410200746A CN103931627B CN 103931627 B CN103931627 B CN 103931627B CN 201410200746 A CN201410200746 A CN 201410200746A CN 103931627 B CN103931627 B CN 103931627B
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- anticorrosion
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Abstract
The present invention relates to a kind of organic blowing agent composite synergistic fungicidal preservative, it is prepared from by 2-methylisothiazolinone and/or 1,2 BITs (BIT) and/or dichloroethenyl salicylamide, sodium pyrithione and/or Sodium hydroxymethyl glycinate, Sodium Dimethyldithiocarbamate and/or orthoxenol, phenylethyl alcohol and/or phenylcarbinol, conditioning agent, solvent and water. The different sterilization and anticorrosion sterilant compounds that the present invention adopts various sterilization spectrum complementary, product have formula rationally, protect strong, the advantage such as sterilization and anticorrosion is effective comprehensive, building performance, in the water-based organic blowing agent containing a large amount of protein and organic polysaccharide, result of use is fine.
Description
Technical field
The invention belongs to the preparing technical field of Chemical Preservation mould inhibitor, it relates to a kind of organic blowing agent composite synergistic fungicidal preservative and its preparation method.
Background technology
Producing in high-performance foam concrete technique, whipping agent is essential material. The whipping agent of high-quality requires to have the advantages such as with low cost, starting material are easy to get, foaming power height and steady bubble time length simultaneously, and the time of particularly surely steeping requires to reach actual service requirements.
Animal proteinum and vegetable-protein whipping agent enter building foaming field so far in a large number. The outstanding advantage that they are owned together is that foam is stable especially, it is possible to the bubble that do not disappear for a long time (its time disappearing bubble completely is longer than 24h mostly), is that the whipping agent of other type cannot mutually when. Therefore, whipping agent domestic at present is substantially taking protein whipping agent as developing direction, as China Patent No. be 201210416023 patent text disclosed in a kind of compound animal/vegetable protein whipping agent, be namely made up of materials such as Unguis Sus domestica, horn powder, dregs of beans, wine groove, polyoxyethylenated alcohol sodium sulfate, Sodium dodecylbenzene sulfonate, tea saponins. But for the whipping agent that animal/vegetable protein is master, owing to it is rich in trophoplasm (protein and sugar), very easily microbial contamination is rotten, the problems such as variable color, flatulence, smelly, precipitation occur, severe patient even loses practical value, and rotten containing the whipping agent of protein after stink very big, almost cannot use, thus also bring problem of environmental pollution. Furthermore user is sometimes in order to improve foaming power, also to be added the natural surface active agents such as soybean phospholipid, tea saponin, black liquid, sugaring raffinate in formula, also make the anticorrosion difficulty of whipping agent increase further. In addition, owing to containing the just very easily microbiological contamination in storage process of protein-based raw material, just having brought microorganism in whipping agent making processes into, making conventional fungicidal preservative consumption much higher, anticorrosion difficulty is very big.
The kind of current known fungicidal preservative is a lot, but yet there are no the fungicidal preservative of highly effective and safe used for the organic blowing agent containing a large amount of protein and sugar class specially on market, generally all with common coating fungicidal preservative substitute. Usual single type fungicidal preservative is very limited for the whipping agent antisepsis and sterilization ability containing a large amount of protein and sugar class, efficiency is very low, this just can be able to judge from its minimum bactericidal concentration (MIC) value, and staging life in summer only will go bad smelly in about ten days, a large amount of putrid and deteriorated cases occurs. Obviously, for the organic blowing agent higher containing protein and sugar class concentration, at all single sanitas to reach desirable preservative effect.
Summary of the invention
It is an object of the invention to be solved by prior art Problems existing, it is provided that a kind of theory has certificate, the organic blowing agent composite synergistic fungicidal preservative that formula is reasonable, cost performance height, sterilization and anticorrosion are effective.
The effective constituent of the organic blowing agent composite synergistic fungicidal preservative provided for realizing foregoing invention object is made up of the raw material of substance of following weight per-cent:
Surplus is water;
Described anticorrosion and bactericidal agent A be selected from following substances one or more: 2-methylisothiazolinone, 1,2 BITs (BIT), dichloroethenyl salicylamide, phenols and salt thereof; Described anticorrosion and bactericidal agent B be selected from following substances one or more: sodium pyrithione, Sodium hydroxymethyl glycinate; Described anticorrosion and bactericidal agent C be selected from following substances one or more: Sodium Dimethyldithiocarbamate, orthoxenol; Described anticorrosion and bactericidal agent D be selected from following substances one or more: phenylethyl alcohol, phenylcarbinol; Described solvent is one or more in following substances: 1,2 propylene glycol, polyoxyethylene glycol, dipropylene glycol, ethylene glycol; Described conditioning agent is alkali metal hydroxide.
Preferred weight part ratio range of the raw material of substance making organic blowing agent composite synergistic fungicidal preservative of the present invention is:
Surplus is water.
The further technical solution of the present invention is also: described anticorrosion and bactericidal agent A is 1,2 BITs (BIT), described anticorrosion and bactericidal agent B is Sodium hydroxymethyl glycinate, and described anticorrosion and bactericidal agent C is orthoxenol, and described anticorrosion and bactericidal agent D is phenylethyl alcohol; Described solvent is polyoxyethylene glycol, dipropylene glycol; Described conditioning agent is sodium hydroxide or potassium hydroxide, is wherein preferably sodium hydroxide.
Method for the preparation of this organic blowing agent composite synergistic fungicidal preservative comprises following processing step:
1, by stirring solvent and be heated to 25 DEG C��30 DEG C, add anticorrosion and bactericidal agent A and stir evenly, adding the conditioning agent accounting for conditioning agent composition weight value 70%��75% subsequently, that anticorrosion and bactericidal agent A is dissolved is complete;
2, deionized water under agitation adding anticorrosion and bactericidal agent C and anticorrosion and bactericidal agent B, the conditioning agent adding surplus gradually makes it dissolve completely;
3, by the solution stirring mixing obtained through step 1 and step 2, add anticorrosion and bactericidal agent D and stir evenly, obtain organic blowing agent composite synergistic fungicidal preservative product.
The useful effect of the present invention as follows described in.
One, the different fungicidal preservative compounds that the present invention adopts various sterilization spectrum complementary, it is made to play fitst water sterilization and anticorrosion effect, and the antimicrobial spectrum according to relevant sanitas realizes having complementary advantages, scientific compatibility forms the compound preservative of the better adaptability that can take into account quick sterilization and long-time Antifungal activity. In pharmaceutical formulation of the present invention, anticorrosion and bactericidal agent C (particularly orthoxenol) activity is very high, and has the sterilization and anticorrosion mildew-resistant ability of wide spectrum, uses its water-soluble and relative comprehensively sterilization and anticorrosion ability at this; Anticorrosion and bactericidal agent A (BIT, dichloroethenyl salicylamide, phenols and salt thereof), then based on kill bacteria, has outstanding antisepsis and sterilization ability when slight alkalinity; Anticorrosion and bactericidal agent B (particularly Sodium hydroxymethyl glycinate) is as excellent low poison sanitas, the antimycotic antiseptics such as starch, coating, spinning sizing agent it are widely used in, at this anticorrosive mildewproof performance utilizing it water-soluble and good when slight alkalinity and the synergetic with other component, it is to increase the security of product; Formula adds anticorrosion and bactericidal agent D (phenylethyl alcohol or phenylcarbinol etc.), the space gas phase sterilization provide protection utilizing it outstanding, the protection domain (space) of sanitas is strengthened; The present invention's solvent (polyoxyethylene glycol or propylene glycol) used is that the organic blowing agent containing protein is had steady bubble effect, can extend the time length of bubble, is also the good solvent of sanitas simultaneously.
Two, using this organic blowing agent composite synergistic fungicidal preservative can reduce the production cost of whipping agent, add-on is far smaller than the add-on in the past adding separately phenol or Sodium Benzoate class fungicidal preservative.
Three, the present invention scientifically by whipping agent system in container anticorrosion with superjacent air space in container is anticorrosion be combined in together with; to the corrosionproof protection that whipping agent material is comprehensive; effectively prevent microorganism from being developed immunity to drugs by sanitas; anticorrosion security and full-scope safeguards height; because many times microorganism growth above container and surface start, especially as mould breeding grow from surface.
Four, the protective system of the present invention and the compatibleness of whipping agent are good, especially at high temperature can directly add (as reached 80��100 DEG C), because selected fungicidal preservative all has resistance to elevated temperatures, this is rarely found in common aseptic applications. Direct high temperature adds and is easily uniformly dispersed, and dissolves rapider, and germ-killing efficiency is higher, reduces temperature fall time simultaneously, saves the energy.
Five, potential of hydrogen (pH value) scope of application of organic blowing agent composite synergistic fungicidal preservative of the present invention is relatively big, neutral best to effect under alkaline condition especially.
Six, the production method of organic blowing agent composite synergistic fungicidal preservative of the present invention is simple, and production cost is low, is easy to realize scale production.
Embodiment
Embodiment 1
The preparation method of a kind of embodiment of organic blowing agent composite synergistic fungicidal preservative of the present invention comprises following processing step:
1, taking BIT10.2 kilogram (BIT12 kilogram of 85%), be dispersed in 35 kilograms of poly(oxyethylene glycol) 400, be stirred and heated to 30 DEG C, 4.5 kilograms, the sodium hydroxide adding 45% makes BIT dissolve, and pH is 9��10;
2, deionized water 10 kilograms under agitation adds the Sodium hydroxymethyl glycinate 16 kilograms of orthoxenol 4 kilograms and 50%, and the aqueous sodium hydroxide solution adding 45% gradually 1.6 kilograms makes it dissolve completely;
3, step 2 and step 1 solution stirring are mixed, add phenylcarbinol 7 kilograms, adding deionized water stirs evenly (if desired by few sodium hydroxide or hydrochloric acid adjusted to ph) to total amount double centner, obtaining a kind of organic blowing agent composite synergistic fungicidal preservative of the present invention, the pH value of this composite synergistic fungicidal preservative is 9.2.
According to organic blowing agent composite synergistic fungicidal preservative prepared by above step, its formula combination is determined through strict microbiological test, mutual building performance experimental study between mainly, and, chamber microbiological challenge is tested and is verified in nearly hundred practical applications in the ground such as Dongguan, Guangdong by experiment, preservative effect is very satisfied, reaches goal of the invention.
The synergism experiment that the mixing microorganisms extracted from production on-site environment and in rotten organic blowing agent does between the antiseptic composition of the present invention more can illustrate problem. Rotten organic blowing agent is carried out microorganism separation and obtains mixed bacterium, these rotten organic blowing agents from North China, East China and south China, the mixed bacterium of major embodiment separation has representative widely. These microorganisms, based on pseudomonas, gas bacillus, are mixed with yeast and mould. Make nutritional medium with tryptic soy broth agar, cultivate 48 hours. Obtain three kinds of sanitass to the minimum bactericidal concentration of production scene mixed bacterium respectively: QA=15 (ppm), QB=25 (ppm), QC=10 (ppm). And when by three kinds of conbined usage, according to the synergy coefficient (SI) that F.C.KU11 etc. sums up, as SI > 1, several sanitas combinationally uses not only can not synergy, and can confront with each other, run counter to desire in other words, add toxicity, reduce the action effect of sanitas, form waste and the infringement to environment; As SI=1, only there is additive effect; Only as SI < 1, just there is synergism, and more big with the difference of 1, and synergism is more strong, and this is also the target pursued in theory. SI=Qa/QA+Qb/QB+Qc/QC��QA��QB��QCBe respectively sanitas A, sanitas B, sanitas C when being used alone to the minimum inhibitory concentration of microorganism. Screen suitable combination and reach the object suppressing to take from the mixing microorganisms of production scene, then have the result of table 1:
Table 1: three kinds of sanitas compound uses are to the synergy killing action of field mix bacterium
This is a part for synergism experiment. The combination that effect is best in theory is: BIT: Sodium hydroxymethyl glycinate: orthoxenol=6:5:1.5; considering price, toxicological security and space protection characteristic (phenylethyl alcohol is space sterilant) obtain the proportionlity between the antiseptic composition of the present invention.
The composite synergistic fungicidal preservative that embodiment 1 is obtained and be used alone phenol or Sodium Benzoate, or BIT, or chlormethylisothiazo,ine ketone and methylisothiazolinone mixture (Kathon CG) carry out the anticorrosion contrast test of normal temperature, follow the tracks of the rotten situation (table 2) of organic blowing agent. Test carries out constant temperature 30 DEG C, produces a large amount of gas, make packaging bulging modification when sample is rotten.
Find composite synergistic fungicidal preservative of the present invention addition be whipping agent quality 0.2% time, the whipping agent quality guaranteed period is more than 180 days; Also never degenerated more than 1 year when add-on is 0.3%. And under same condition, it is no more than 50 days with whipping agent quality guaranteed period during other sanitas, the shortest also with regard to 10 days. Visible, the sterilization and anticorrosion effect of composite synergistic fungicidal preservative of the present invention is ideal, considerably beyond the sterilization and anticorrosion ability of conventional sanitas.
Table 2: synergy compound preservative of the present invention and the contrast of other sanitas usefulness
Embodiment 2
The preparation method of another kind of embodiment of organic blowing agent composite synergistic fungicidal preservative of the present invention comprises following processing step:
1, taking BIT12 kilogram (BIT14.1 kilogram of 85%), be dispersed in the 1,2-propylene glycol of 40 kilograms, be stirred and heated to 30 DEG C, 5.5 kilograms, the sodium hydroxide adding 45% makes BIT dissolve, and pH is 9��10;
2, deionized water 10 kilograms under agitation adds the Sodium hydroxymethyl glycinate 14 kilograms of orthoxenol 5 kilograms and 50%, and the aqueous sodium hydroxide solution adding 45% gradually 1.9 kilograms makes it dissolve completely;
3, step 2 and step 1 solution stirring are mixed, add phenylcarbinol 8 kilograms, adding deionized water stirs evenly (if desired by few sodium hydroxide or hydrochloric acid adjusted to ph) to total amount double centner, obtaining another kind of organic blowing agent composite synergistic fungicidal preservative of the present invention, the pH value of this compound preservative is 9.5.
Composite synergistic fungicidal preservative embodiment 2 obtained is used for the SH-126 high efficiency composition water chestnut magnesium organic blowing agent product that is produced from Dongguan, it is mixed bacterium to the bacterial classification wherein added, comprise Pseudomonas aeruginosa, streptococcus aureus, intestinal bacteria, Candida albicans bacterium, black-koji mould, penicillium funiculosum, viride, 37 DEG C of constant temperature culture 28 days, the growth and breeding situation of periodic detection wherein bacterium and mould, provides challenge test-results (table 3) after 28 days. Test concentrations: sanitas add-on 0.3%. In addition, practical application also shows, the add-on of 0.3% can make organic blowing agent preserve under hot and humid condition to never degenerate for 4 months.
Mixing microorganisms challenge is tested by table 3 composite synergistic fungicidal preservative 0.3% of the present invention
Claims (3)
1. an organic blowing agent composite synergistic fungicidal preservative, it is characterised in that the effective constituent of this composite synergistic fungicidal preservative is made up of the raw material of substance of following weight per-cent:
Described anticorrosion and bactericidal agent A is 1,2 BITs; Described anticorrosion and bactericidal agent B is Sodium hydroxymethyl glycinate; Described anticorrosion and bactericidal agent C is orthoxenol; Described anticorrosion and bactericidal agent D is phenylcarbinol; Described solvent is polyoxyethylene glycol; Described conditioning agent is sodium hydroxide.
2. an organic blowing agent composite synergistic fungicidal preservative, it is characterised in that the effective constituent of this composite synergistic fungicidal preservative is made up of the raw material of substance of following weight per-cent:
Described anticorrosion and bactericidal agent A is 1,2 BITs; Described anticorrosion and bactericidal agent B is Sodium hydroxymethyl glycinate; Described anticorrosion and bactericidal agent C is orthoxenol; Described anticorrosion and bactericidal agent D is phenylcarbinol; Described solvent is 1,2-propylene glycol; Described conditioning agent is sodium hydroxide.
3. one kind for the preparation of the method for organic blowing agent described in claim 1 or 2 with composite synergistic fungicidal preservative, it is characterised in that comprises following processing step:
Step 1: by stirring solvent and be heated to 30 DEG C, add anticorrosion and bactericidal agent A and stir evenly, the conditioning agent adding part value subsequently makes anticorrosion and bactericidal agent A dissolve completely, and the weight being added conditioning agent accounts for the 70%��75% of conditioning agent component weight value;
Step 2: agitating deionized water, adds anticorrosion and bactericidal agent C and anticorrosion and bactericidal agent B wherein, and the conditioning agent adding surplus gradually makes it dissolve completely;
Step 3: by the solution stirring mixing obtained through step 1 and step 2, add anticorrosion and bactericidal agent D and stir evenly, obtain organic blowing agent composite synergistic fungicidal preservative product.
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| JP6275063B2 (en) * | 2015-02-03 | 2018-02-07 | ライオン株式会社 | Living space treatment agent for piezo-type sprayer |
| WO2016196116A1 (en) * | 2015-05-31 | 2016-12-08 | Dow Global Technologies Llc | Microbicidal composition containing ortophenylphenol and isothiazolinone |
| CN108486956A (en) * | 2018-06-26 | 2018-09-04 | 潍坊科技学院 | A kind of special type papermaking Compositional type mould inhibitor |
| CN109704624A (en) * | 2018-11-27 | 2019-05-03 | 天津城建大学 | A kind of microorganism foaming agent and preparation method for foamed concrete preparation |
| CN112773780A (en) * | 2019-11-11 | 2021-05-11 | 深圳优丽康生物技术有限公司 | Composition for vagina and vulva and application thereof |
| CN113994969B (en) * | 2021-10-26 | 2023-10-13 | 上海迈肯生物科技有限公司 | Sodium pyrithione compound preservative, preparation method and application thereof |
| CN114231119B (en) * | 2021-11-24 | 2023-07-07 | 中山大学 | Preparation method and application of anti-corrosion and anti-fouling integrated coating with self-repairing function |
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| DE102005022148A1 (en) * | 2005-05-13 | 2006-11-23 | Lanxess Deutschland Gmbh | Fungicidal mixtures |
| EP1964541A1 (en) * | 2007-03-02 | 2008-09-03 | Takasago International Corporation | Preservative compositions |
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| CN102702839B (en) * | 2012-06-29 | 2014-02-12 | 陕西省石油化工研究设计院 | In-tank antiseptic antimildew agent composition integrated with dry film for paint |
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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 |