CN103918709A - Preparation method of high-efficiency composite antibacterial and mildew-proof organic-silicon quaternary ammonium salt reagent - Google Patents

Preparation method of high-efficiency composite antibacterial and mildew-proof organic-silicon quaternary ammonium salt reagent Download PDF

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Publication number
CN103918709A
CN103918709A CN201410167599.8A CN201410167599A CN103918709A CN 103918709 A CN103918709 A CN 103918709A CN 201410167599 A CN201410167599 A CN 201410167599A CN 103918709 A CN103918709 A CN 103918709A
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China
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quaternary ammonium
ammonium salt
solution
preparation
organic silicon
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CN201410167599.8A
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周涛
周宇鹏
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NANXIONG TRIPOD CHEMICAL Co Ltd
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NANXIONG TRIPOD CHEMICAL Co Ltd
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Abstract

The invention relates to a preparation method of a high-efficiency composite antibacterial and mildew-proof organic silicon quaternary ammonium salt reagent. The preparation method comprises the following processing steps: firstly adding organic silicon quaternary ammonium salt solution to isopropyl alcohol to prepare isopropyl alcohol solution containing organic silicon quaternary ammonium salt with the weight ratio of 60%, pouring 72% of organic silicon quaternary ammonium salt into a container, adding isopropyl alcohol into the container under stirring, and carrying out preheating stirring so as to fully dissolve the organic silicon quaternary ammonium salt and the isopropyl alcohol to form uniform and transparent 60% organic silicon quaternary ammonium salt antibacterial reagent solution; then adding 7.35kg of 98% 2-octyl-2H-isothiazol-3-one into 4.9kg of propylene glycol, and uniformly stirring to form 60% 2-Octyl-2H-isothiazol-3-one propylene glycol solution; finally pouring 60% 2-Octyl-2H-isothiazol-3-one propylene glycol solution to 60% of organic silicon quaternary ammonium salt antibacterial reagent solution under stirring so as to obtain a composite antibacterial and mildew-proof reagent. The preparation method has the characteristics of small application amount, good compatibility and low toxicity, and can be applied to antibacterial and mildew-proof treatment of leather, fabric, coating and various building materials.

Description

A kind of preparation method of efficient composite organic quaternary ammonium salt antibacterial mildew inhibitor
Technical field
The invention belongs to antibacterial mildew inhibitor technical field, relate to a kind of preparation method of efficient composite organic quaternary ammonium salt antibacterial mildew inhibitor.
Background technology
Organosilicon quaternary ammonium salt is as silica-based in 3-(tri-alkoxy) propyl group octadecyl alkyl dimethyl ammonium chloride is the durable washable antibacterial agent that last century, the seventies was invented by Dow corning company, trade name DC-5700.Because there being quaternary ammonium salt cationic gene on its molecule, various bacteriums are had to good antibacterial and bacteriostasis as Escherichia coli and to various fungies as gram-positive bacteria, staphylococcus aureus and Gram-negative bacteria.Alcoxyl its (methoxy or ethoxy) because containing three facile hydrolysis on its molecule again, under the effect of water, facile hydrolysis is three silicon hydroxyls, the easy polycondensation under acid, alkali effect of silicon hydroxyl is space network, make silicon quaternary ammonium salt water insoluble, be attached to securely base material (as fabric, leather, timber) upper, thus play durable antibacterial action.But because organosilicon quaternary ammonium salt molecular weight is larger, the quantitative quaternary ammonium group of unit is few, so antibacterial agent large usage quantity, detect through authoritative institution, organosilicon quaternary ammonium salt to the minimum inhibitory concentration of various bacteriums more than 200PPM, in practical application, for prevent the growth of various moulds under adverse circumstances, the consumption of organosilicon quaternary ammonium salt is just insurance more than 1%.This is non-remunerative economically.
Chinese Patent Application No. 20131078618.2 adopts shitosan and organosilicon quaternary ammonium salt complex antimicrobials for anti-inflammation, and the anti-microbial property of shitosan is strong not; Chinese Patent Application No. 201210165355.7 adopts organosilicon quaternary ammonium salt and nano-titanium dioxide composite antibacterial agent to process bafta, and nano titanium oxide has catalytic action, and antibacterial agent ageing-resistant performance is reduced; The patent of people's applications such as Henan Lee Bi Zhong adopts Nano Silver, organosilicon quaternary ammonium salt and octyl group thiazolinone are the antiviral inorganic agent of composite antibacterial, first influenza virus and avian influenza virus are had to good insect killing effect, but must be durable by emulsion acrylic resin adhesive ability, and the easy oxidation stain of Nano Silver, finally become grey black, and expensive.
Summary of the invention
For overcoming above-mentioned technical disadvantages, the invention provides a kind of preparation method who utilizes organosilicon quaternary ammonium salt and octyl group isothiazolinone to be prepared into a kind of efficient composite organic quaternary ammonium salt antibacterial mildew inhibitor, can be applicable to leather, fabric, the antibacterial and mouldproof processing of coating and various building materials, have that application quantity is little, compatibility good, the feature that toxicity is low.
The present invention solves the technical method that its technical problem adopts: a kind of preparation method of efficient composite organic quaternary ammonium salt antibacterial mildew inhibitor, and its processing step is:
A. 72% organosilicon quaternary ammonium salt solution being added isopropyl alcohol to be made into machine silicon quaternary ammonium salt, to contain weight ratio be 60% aqueous isopropanol: take 72% organosilicon quaternary ammonium salt 100kg and pour in container, and under agitation in container, add isopropyl alcohol 20kg, be preheated to 30 DEG C~40 DEG C, stir 10min~20min, make it fully be dissolved into 60% silicone Quaternary Ammonium Salt Antimicrobial Agent solution of homogeneous transparent;
B, 98% octyl group isothiazolinone 7.35kg is added in the propane diols of 4.9kg, is stirred into 60% the different thiophene quinoline of octyl group ketone propylene glycol solution;
C, under agitation, different 60% octyl group thiophene quinoline ketone propylene glycol solution is poured in 60% silicone Quaternary Ammonium Salt Antimicrobial Agent solution, weight ratio is 1:10, obtains composite antimicrobial mould inhibitor, in composite antimicrobial mould inhibitor solution, contains the different thiophene quinoline of octyl group ketone 5.6% containing organosilicon quaternary ammonium salt 54.4%.
In described A step, container used is porcelain enamel barrel, and agitator is the dasher of portable electric tetrafluoroethene cladding, and the rotating speed of agitator is 100 r/min~800r/min;
Octyl group isothiazolinone in described B step adopts Dalian Bio-Chem Co., Ltd. to produce.
Beneficial effect of the present invention: have that application quantity is little, compatibility good, the feature that toxicity is low, can be applicable to leather, fabric, the antibacterial and mouldproof processing of coating and various building materials.
embodiment
Below in conjunction with embodiment, the present invention is further described.
A preparation method for efficient composite organic quaternary ammonium salt antibacterial mildew inhibitor, its processing step is:
A. 72% organosilicon quaternary ammonium salt solution being added isopropyl alcohol to be made into machine silicon quaternary ammonium salt, to contain weight ratio be 60% aqueous isopropanol: take 72% organosilicon quaternary ammonium salt 100kg and pour in container, and under agitation in container, add isopropyl alcohol 20kg, be preheated to 30 DEG C~40 DEG C, stir 10min~20min, make it fully be dissolved into 60% silicone Quaternary Ammonium Salt Antimicrobial Agent solution of homogeneous transparent;
B, 98% octyl group isothiazolinone 7.35kg is added in the propane diols of 4.9kg, is stirred into 60% the different thiophene quinoline of octyl group ketone propylene glycol solution;
C, under agitation, pours different 60% octyl group thiophene quinoline ketone propylene glycol solution in 60% silicone Quaternary Ammonium Salt Antimicrobial Agent solution, obtains composite antimicrobial mould inhibitor, in composite antimicrobial mould inhibitor solution containing organosilicon quaternary ammonium salt 54.4% containing the different thiophene quinoline of octyl group ketone 5.6%.
In described A step, container used is porcelain enamel barrel, and agitator is the dasher of portable electric tetrafluoroethene cladding, and the rotating speed of agitator is 100 r/min~800r/min;
Octyl group isothiazolinone in described B step adopts Dalian Bio-Chem Co., Ltd. to produce.
Embodiment 1: preparation and the application of spraying working solution, taking ethanol as the molten antibacterial and mouldproof working solution that is made into any concentration of dilution, object is to be convenient to be applied to easily dry fur, and woollen blanket, on the layer such as carpet and stone material, as the formulation content aerial fog type spray mould inhibitor that is 0.6%, in enamelled vessel, add absolute ethyl alcohol 99kg, under agitation add 60% composite antimicrobial mould inhibitor 1kg, adjusting pH value with acetic acid is afterwards 6.0 ~ 7.0 to obtain the aerosol solution that 100kg composite antimicrobial mould inhibitor content is 0.6%, can be used for leather, fur, the spraying mildew-resistant processing of carpet, in aerosol, contain compound anti-mist agent 6000PPM.
Embodiment 2: do not add 60% composite antimicrobial mould inhibitor 1kg in (electrical conductivity≤5 × 10.4s/m) at 99kg deionization, the available water that stirs acetic acid adjust pH 5.0~7.0, just obtain the water mildow-proof agent containing composite mildew inhibitor 6000PPM, this aqueous solution shelf stable for periods, can spraying or dip-coating or brush to timber, paper, fabric face, dry or dry and just obtain durable mold proof product more than 1 year.
Embodiment 3: be applied to oil paint, first to determine it is the paint of any type, there is ethanol-soluble type as alcohol acids paints, just, as long as add paint to account for 1%~3% of paint total amount 60% composite antimicrobial mould inhibitor solution, fully stir evenly, if not alcohol-soluble resin paint, will use cellosolve, as butyl glycol ether class, propane diols ethers, after 2~3 times of carbonates or toluene class solution dilution antibacterial mildew inhibitors, join in paint and fully stir evenly again, dosage is 1%~3% of paint total amount.
Embodiment 4: composite antimicrobial mould inhibitor is applied in water paint, the large multiplex polymer emulsion of water paint, as poly-acetic acid second dilute emulsion, ethene~acetate copolymer emulsion, propylene vinegar copolymer emulsion, Polyurethane emulsion etc. is done film forming matter.This class emulsion is nonionic or anionic emulsion mostly, and nonionic emulsion has no adverse effects to silicone Quaternary Ammonium Salt Antimicrobial Agent.If anionic emulsion wherein anion surfactant the antibacterial effect of organosilicon quaternary ammonium salt is had to certain negative function; at this moment be preferably in before coating application first and first spray one or brush once with 1%~2% the composite antimicrobial mould inhibitor aqueous solution; after surface dry, be coated with again water paint; ensure base material mildew-resistant; make again the mildew-resistant of resin film forming matter protection bottom be difficult for loss, make mildew-resistant more durable.
The present invention has that application quantity is little, compatibility good, and the feature that toxicity is low, can be applicable to leather, fabric, the antibacterial and mouldproof processing of coating and various building materials.

Claims (3)

1. a preparation method for efficient composite organic quaternary ammonium salt antibacterial mildew inhibitor, is characterized in that processing step is:
A. 72% organosilicon quaternary ammonium salt solution being added isopropyl alcohol to be made into machine silicon quaternary ammonium salt, to contain weight ratio be 60% aqueous isopropanol, taking 72% organosilicon quaternary ammonium salt 100kg pours in container, and under agitation in container, add isopropyl alcohol 20kg, be preheated to 30 DEG C~40 DEG C, stir 10min~20min, make it fully be dissolved into 60% silicone Quaternary Ammonium Salt Antimicrobial Agent solution of homogeneous transparent;
B, 98% octyl group isothiazolinone 7.35kg is added in the propane diols of 4.9kg, is stirred into 60% the different thiophene quinoline of octyl group ketone propylene glycol solution;
C, under agitation, different 60% octyl group thiophene quinoline ketone propylene glycol solution is poured in 60% silicone Quaternary Ammonium Salt Antimicrobial Agent solution, weight ratio is 1:10, obtains composite antimicrobial mould inhibitor, in composite antimicrobial mould inhibitor solution, contains the different thiophene quinoline of octyl group ketone 5.6% containing organosilicon quaternary ammonium salt 54.4%.
2. the preparation method of efficient composite organic quaternary ammonium salt antibacterial mildew inhibitor as claimed in claim 1: it is characterized in that: in described A step, container used is porcelain enamel barrel, agitator is the dasher of portable electric tetrafluoroethene cladding, and the rotating speed of agitator is 100 r/min~800r/min.
3. the preparation method of efficient composite organic quaternary ammonium salt antibacterial mildew inhibitor as claimed in claim 1: the octyl group isothiazolinone in described B step adopts Dalian Bio-Chem Co., Ltd. to produce.
CN201410167599.8A 2014-04-24 2014-04-24 Preparation method of high-efficiency composite antibacterial and mildew-proof organic-silicon quaternary ammonium salt reagent Pending CN103918709A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104974636A (en) * 2015-06-23 2015-10-14 安徽华辉塑业科技有限公司 Environment-friendly antibacterial and antifungal powder coating and preparation method therefor
CN105638721A (en) * 2016-03-26 2016-06-08 广州佳伲思抗菌材料有限公司 Mildew prevention and removal agent for textiles and leather products
CN105831148A (en) * 2016-03-26 2016-08-10 广州佳伲思抗菌材料有限公司 Fungicide for water-based glue, preparation method and application thereof
CN106172434B (en) * 2016-06-27 2018-08-21 宁德师范学院 A kind of wall clothing biocide mildewcide and preparation method thereof
CN110157294A (en) * 2019-05-28 2019-08-23 六安科瑞达新型材料有限公司 A kind of antibacterial powder paint
CN113248891A (en) * 2020-02-11 2021-08-13 吉林金源北方科技发展有限公司 Composite antibacterial material based on carbon dioxide copolymer and preparation method thereof
CN113529415A (en) * 2021-08-12 2021-10-22 杭州锴越新材料有限公司 Antibiotic mould proof seam plaiting cloth
CN114085608A (en) * 2021-12-30 2022-02-25 佛山阳光逸采涂料科技有限公司 Water-based ultraviolet light-cured antiviral coating and preparation method and application thereof

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CN102296465A (en) * 2010-12-30 2011-12-28 上海水星家用纺织品股份有限公司 Cassia seed composite antibacterial finishing agent, preparation method, method for processing fiber and application
CN102669179A (en) * 2012-05-30 2012-09-19 北京崇高纳米科技有限公司 Antibacterial antiviral treating agent, preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102296465A (en) * 2010-12-30 2011-12-28 上海水星家用纺织品股份有限公司 Cassia seed composite antibacterial finishing agent, preparation method, method for processing fiber and application
CN102669179A (en) * 2012-05-30 2012-09-19 北京崇高纳米科技有限公司 Antibacterial antiviral treating agent, preparation method and application thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104974636A (en) * 2015-06-23 2015-10-14 安徽华辉塑业科技有限公司 Environment-friendly antibacterial and antifungal powder coating and preparation method therefor
CN105638721A (en) * 2016-03-26 2016-06-08 广州佳伲思抗菌材料有限公司 Mildew prevention and removal agent for textiles and leather products
CN105831148A (en) * 2016-03-26 2016-08-10 广州佳伲思抗菌材料有限公司 Fungicide for water-based glue, preparation method and application thereof
CN106172434B (en) * 2016-06-27 2018-08-21 宁德师范学院 A kind of wall clothing biocide mildewcide and preparation method thereof
CN110157294A (en) * 2019-05-28 2019-08-23 六安科瑞达新型材料有限公司 A kind of antibacterial powder paint
CN110157294B (en) * 2019-05-28 2021-01-29 六安科瑞达新型材料有限公司 Antibacterial powder coating
CN113248891A (en) * 2020-02-11 2021-08-13 吉林金源北方科技发展有限公司 Composite antibacterial material based on carbon dioxide copolymer and preparation method thereof
CN113529415A (en) * 2021-08-12 2021-10-22 杭州锴越新材料有限公司 Antibiotic mould proof seam plaiting cloth
CN114085608A (en) * 2021-12-30 2022-02-25 佛山阳光逸采涂料科技有限公司 Water-based ultraviolet light-cured antiviral coating and preparation method and application thereof

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Application publication date: 20140716