CN106317448A - Preparation method of color-changeable antibacterial sponge - Google Patents

Preparation method of color-changeable antibacterial sponge Download PDF

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CN106317448A
CN106317448A CN201610706013.XA CN201610706013A CN106317448A CN 106317448 A CN106317448 A CN 106317448A CN 201610706013 A CN201610706013 A CN 201610706013A CN 106317448 A CN106317448 A CN 106317448A
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sponge
color
step
agent
solvent
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CN201610706013.XA
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CN106317448B (en
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陈艾刚
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盐城市天马日用品有限公司
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/36After-treatment
    • C08J9/40Impregnation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/36After-treatment
    • C08J9/40Impregnation
    • C08J9/42Impregnation with macromolecular compounds

Abstract

The invention discloses a preparation method of color-changeable antibacterial sponge. The preparation method comprises the following steps: (1) dissolving and diluting a colorless antibacterial agent and a pigment on the market with a solvent A to a specified proportion, heating to 40 to 75 DEG C under a condition of nitrogen sealing, adjusting the PH value, slowly dripping a coupling agent, preserving the heat for 2 to 5 h at the end of dripping, diluting a sample with the solvent A, and determining that the sample is qualified if no precipitate is produced; (2) heating the solution obtained in the step (1), stabilizing the temperature to 70 to 90 DEG C, slowly dripping a slow release color fixing agent, controlling a reflux speed, further preserving the heat for 2 to 5 h at the end of reaction, adjusting the PH value, diluting a sample with the solvent A, and determining that the sample is qualified if no precipitate is produced; (3) uniformly mixing the colored antibacterial agent solution obtained in the step (2) and an adhesive according to a proportion to obtain a mixture, and soaking and drying with colored sponge after the mixture is thickened so as to prepare the color-changeable antibacterial sponge. The production process is reasonable, and the operability is high; the prepared antibacterial sponge is long in bacterium resisting time, can be discolored, and is high in practicability.

Description

一种可变色抗菌海绵的制备方法 A method of preparing an antimicrobial sponge discoloration

技术领域 FIELD

[0001]本发明涉及一种海绵的制备方法,具体涉及一种具有持续抗菌活性的可变色海绵的制备方法。 [0001] The present invention relates to a method of preparing a method for sponge, particularly relates to a sustained antimicrobial activity may be discolored sponge.

背景技术 Background technique

[0002]目前国内外市场上现有抗菌海绵都是采用生产海绵过程中加入抗菌剂的工艺生产海绵,具有一定的抗菌效果,但是抗菌性能的稳定性较差,且分散不均匀,随着使用时间延长,抗菌效果越来越差,不能确认有无抗菌效果,实用性不强。 [0002] Currently on the market and abroad using conventional antimicrobial sponge are added during the production of sponge antimicrobial sponge production process, a certain antimicrobial effect, antibacterial properties but poor stability, and non-uniform dispersion, with the use of prolonged antimicrobial effect is getting worse, can not confirm whether or antibacterial effect, practicality is not strong.

发明内容 SUMMARY

[0003]发明目的:本发明的目的是为了解决现有技术的不足,提供一种生产工艺合理,可操作性强的可变色的抗菌海绵的制备方法。 [0003] Object of the invention: object of the present invention is to solve the deficiencies of the prior art, provides a method for producing a reasonable process, operable discoloration may antimicrobial sponge. 该方法能使抗菌剂均匀分散,抗菌时间长,并在抗菌剂中耦合环保色素,控制抗菌剂释放速度,随着使用时间加长,抗菌剂含量逐步减少,而呈现海绵颜色渐变,当抗菌效果达不到标准时最终突变成另外一个颜色的海绵,实用性强。 This method enables the uniform dispersion of the antimicrobial agent, the antimicrobial long time, and green pigments coupling antimicrobial agent, the release rate controlling antimicrobial agent, with the use of longer, gradually reduce the content of an antibacterial agent, a color gradient is presented sponge, when the antibacterial effect of the final color of a further mutation into a sponge with less than standard, practical.

[0004]技术方案:为了实现以上目的,本发明采取的技术方案为: [0004] Technical Solution: To achieve the above object, the present invention takes technical solutions:

[0005] —种可变色海绵的制备方法,其特征在于,包括以下步骤: [0005] - preparation methods can be color sponge, characterized by comprising the steps of:

[0006] (I)取无色抗菌剂、颜料用溶剂A溶解稀释,在氮封的条件下,升温温到40〜75°C,调节PH值,缓慢滴加耦合剂,控制反应温度,滴加结束后保温2〜5小时,取反应产物静置不分层,再用溶剂A稀释无沉淀物; [0006] (I) taken as a colorless antibacterial agent, a pigment is dissolved diluted with a solvent A, at a nitrogen blanket, and heated to a temperature of 40~75 ° C, adjusting the PH value of the coupling agent was slowly added dropwise, controlling the reaction temperature, dropwise after adding 2 ~ 5 hours incubation, the reaction product was allowed to stand taken not hierarchical, then diluted with a solvent A precipitate;

[0007] (2)取步骤(I)溶液加热并恒温到70〜90°C,缓慢滴加缓释型固色剂,控制回流反应速度,避免突沸冲料,滴加结束后,在无回流情况下,继续保温2〜5小时,调节PH值,取回流反应产物,静置不分层,用溶剂A稀释无沉淀物; [0007] (2) from step (I) and the temperature was heated to 70~90 ° C, was slowly added dropwise release fixative, control the reaction rate at reflux, to avoid bumping red material, after the completion of dropping, in the absence of reflux case, incubation was continued for 2 ~ 5 hours, adjusting the PH value of the reaction product stream retrieval, non-hierarchical standing, no precipitate was diluted with a solvent A;

[0008] (3)取步骤(2)带色抗菌剂溶液和粘结剂按比例混合均匀,增稠后用彩色海绵浸渍烘干即制成可变色的抗菌海绵。 [0008] (3) from step (2) colored antimicrobial agent and a binder solution was mixed uniformly, i.e. drying after thickening can be made with a color color antimicrobial sponge impregnated sponge.

[0009]作为优选方案,以上所述的可变色海绵的制备方法,步骤(I)所述的无色抗菌剂为有机抗菌剂,例如有机锌类;颜料为有机颜料,例如酞菁蓝类;溶剂A为能和醇、酮类溶剂及树脂类粘结剂互溶的有机溶剂,例如多元醇类,如丙三醇。 [0009] As a preferred embodiment, the above method of preparation of the sponge may be discolored, said step (I) as a colorless antimicrobial agent is an organic antimicrobial agent, for example, organic zinc-based; the pigment is an organic pigment such as phthalocyanine blue type; solvent a was able and alcohol, ketone solvent and a binder resin miscible organic solvents, such as polyhydric alcohols, such as glycerol.

[0010]作为优选方案,以上所述的可变色海绵的制备方法,其特征在于,步骤(I)调节PH值7〜10,反应温度为40〜75°C。 [0010] As a preferred embodiment, the above method of preparation of the sponge may be discolored, wherein step (I) adjusting the PH value of 7 to 10, the reaction temperature is 40~75 ° C.

[0011]作为优选方案,以上所述的可变色海绵的制备方法,其特征在于,步骤(2)所述的固色剂为改性丙烯酸酯类聚合物,调节PH值为7〜10 [0011] As a preferred embodiment, color can be prepared according to the above sponge, wherein the step (2) of the fixing agent is a modified acrylic polymer, adjusting the PH value of 7 to 10

[0012]作为优选方案,以上所述的可变色海绵的制备方法,其特征在于,步骤(3)带色抗菌剂为有机抗菌剂,颜料为有机颜料,粘结剂为改性丙烯酸酯类聚合物。 [0012] As a preferred embodiment, color can be prepared according to the above sponge, wherein the step (3) the antimicrobial agent is colored organic antibacterial agents, pigment is an organic pigment, the binder is a modified acrylate-based polymerizable thereof.

[0013]作为优选方案,以上所述的可变色海绵的制备方法,其特征在于,步骤(3)带色抗菌剂溶液和粘结剂混合重量比为:0.5〜5: 5〜20。 [0013] As a preferred embodiment, the above method of preparation of the sponge may be discolored, wherein, in step (3) colored antimicrobial solution, and a binder in a weight ratio: 0.5~5: 5~20.

[0014]有益效果:本发明提供的可变色抗菌海绵的制备方法和现有技术相比具有以下优占.V. [0014] Advantageous Effects: The present invention provides an antimicrobial sponge may be discolored and preparation prior art has the following advantages compared to account .V.

[0015]本发明提供的可变色抗菌海绵的制备方法的制备方法,生产工艺合理,可操作性强,通过大量实验筛选出各原料的最佳组成、配比和最佳的反应条件。 [0015] A method for preparing an antimicrobial sponge may color the present invention provides a reasonable production process, easy to operate, screened by the large number of experiments the optimum composition of each raw material, ratio and optimum reaction conditions. 该方法能使抗菌剂均匀分散,抗菌时间长,并在抗菌剂中耦合环保色素,控制抗菌剂释放速度,随着使用时间加长,抗菌剂含量逐步减少,而呈现海绵颜色渐变,当抗菌效果达不到标准时最终突变成另外一个颜色的海绵,实用性强。 This method enables the uniform dispersion of the antimicrobial agent, the antimicrobial long time, and green pigments coupling antimicrobial agent, the release rate controlling antimicrobial agent, with the use of longer, gradually reduce the content of an antibacterial agent, a color gradient is presented sponge, when the antibacterial effect of the final color of a further mutation into a sponge with less than standard, practical.

具体实施方式 Detailed ways

[0016]下面结合具体实施例,进一步阐明本发明,应理解这些实施例仅用于说明本发明而不用于限制本发明的范围,在阅读了本发明之后,本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定的范围。 [0016] The following embodiments with reference to specific embodiments, further illustrate the present invention, it should be understood that these embodiments are illustrative only and the present invention is not intended to limit the scope of the present invention, after reading this disclosure, those skilled in the art of the various invention the modifications are equivalents fall within the present application as defined by the appended claims scope.

[0017]以下实施例所用的无水乙醇、正硅酸四乙酯、氨水皆为分析纯,水用实验室自制的超纯水。 [0017] The following example is used ethanol embodiment, tetraethyl orthosilicate, aqueous ammonia are all analytical grade, made with ultrapure water laboratory.

[0018] 实施例1 [0018] Example 1

[0019 ] —种可变色抗菌海绵的制备方法,其特征在于,包括以下步骤: [0019] - method of producing an antimicrobial sponge may be discolored, which is characterized by comprising the steps of:

[0020] (I)取无色抗菌剂和颜料,用溶剂A溶解稀释,在氮封的条件下,升温到75°C,调节PH值为8,缓慢滴加硅烷耦合剂,控制反应温度450C,滴加结束后保温3小时,取反应物,静置不分层,再用溶剂A稀释至无沉淀物; [0020] (I) taken as a colorless pigment and an antibacterial agent, dissolved diluted with a solvent A, at a nitrogen blanket, and heated to 75 ° C, adjusting the PH value of 8, a silane coupling agent was slowly added dropwise, controlling the reaction temperature 450C after dropping was completed for 3 hours, the reaction was taken, allowed to stand non-hierarchical, non-diluted with solvent A to precipitate;

[0021] (2)取步骤(I)溶液加热并恒温到80°C,缓慢滴加缓释型固色剂改性丙烯酸酯类聚合物,控制回流速度,避免突沸冲料,滴加结束后,在无回流情况下,继续保温3小时,调节PH值为8,取样,静置不分层,用溶剂A稀释无沉淀物,制得的带色抗菌剂溶液; [0021] (2) from step (I) and the temperature was heated to 80 ° C, was slowly added dropwise release fixative modified acrylic polymer, and the reflux rate control to avoid bumping red material, after the completion of the dropping , in the absence of reflux continued for 3 hours, adjusting the PH value of 8, sampling, non-hierarchical standing, no precipitate was diluted with solvent a, the obtained colored antimicrobial solution;

[0022] (3)取步骤(2)制得的带色抗菌剂溶液和粘结剂丙烯酸酯类聚合物按比例混合均匀,增稠后用普通彩色海绵浸渍,烘干,制成可变色的抗菌海绵。 [0022] (3) from step (2) obtained colored antimicrobial agent and a binder solution of an acrylic polymer was mixed uniformly, after thickening with a normal color sponge soaking, drying, discoloration can be made antibacterial sponge.

[0023]以上所述的可变色海绵的制备方法,步骤(I)所述的无色抗菌剂为有机抗菌剂,如有机锌类,颜料为酞菁蓝类有机颜料,溶剂A为丙三醇。 [0023] The method described above may be prepared sponge color, step (I) of the antimicrobial agent is a colorless organic antimicrobial agent, such as zinc-based organic pigment is a phthalocyanine-based blue organic pigment, solvent A is glycerol .

[0024]以上所述的可变色海绵的制备方法,步骤(3)带色抗菌剂溶液和粘结剂重量比例为5:10。 [0024] The method described above may be prepared sponge color, step (3) colored antimicrobial agent solution and the binder weight ratio of 5:10.

[0025] 实施例2 [0025] Example 2

[0026] —种可变色抗菌海绵的制备方法,其特征在于,包括以下步骤: [0026] - method of producing an antimicrobial sponge may be discolored, which is characterized by comprising the steps of:

[0027] (I)取无色抗菌剂和颜料,用溶剂A溶解稀释,在氮封的条件下,升温到55°C,调节PH值为10,缓慢滴加硅烷耦合剂,控制反应温度750C,滴加结束后保温2小时,取反应物,静置不分层,再用为溶剂A稀释至无沉淀物; [0027] (I) taken as a colorless pigment and an antibacterial agent, dissolved diluted with a solvent A, at a nitrogen blanket, and warmed to 55 ° C, adjusting the PH value of 10, a silane coupling agent was slowly added dropwise, controlling the reaction temperature 750C after completion of the dropping for 2 hours, the reaction was taken, allowed to stand non-hierarchical, and diluted with a solvent to precipitate non-A;

[0028] (2)取步骤(I)溶液加热并恒温到70°C,缓慢滴加缓释型固色剂改性丙烯酸酯类聚合物,控制回流速度,避免突沸冲料,滴加结束后,在无回流情况下,继续保温4小时,调节PH值为10,取样,静置不分层,用溶剂A稀释无沉淀物,制得的带色抗菌剂溶液; [0028] (2) from step (I) and the temperature was heated to 70 ° C, was slowly added dropwise release fixative modified acrylic polymer, and the reflux rate control to avoid bumping red material, after the completion of the dropping , in the absence of reflux continued for 4 hours, adjusting the PH value of 10, sampling, non-hierarchical standing, no precipitate was diluted with solvent a, the obtained colored antimicrobial solution;

[0029] (3)取步骤(2)制得的带色抗菌剂溶液和粘结剂按比例混合均匀,增稠后用普通彩色海绵浸渍,烘干,制成可变色的抗菌海绵。 [0029] (3) from step (2) obtained colored antimicrobial agent and a binder solution was mixed in proportion, after thickening with a normal color sponge soaking, drying, discoloration can be made antimicrobial sponge.

[0030]以上所述的可变色海绵的制备方法,步骤(I)所述的可变色海绵的制备方法,步骤(I)所述的无色抗菌剂为有机抗菌剂,如有机锌类,颜料为酞菁蓝类有机颜料,溶剂A为丙三醇。 [0030] The method described above may be prepared sponge color, step (I) can be prepared according to color sponge, the step (I) of the antimicrobial agent is a colorless organic antimicrobial agent, such as an organozinc, pigments phthalocyanine-based blue organic pigment, solvent A is glycerol.

[0031]以上所述的可变色海绵的制备方法,其特征在于,步骤(3)所述的粘结剂为丙烯酸酯类聚合物。 [0031] The method described above may be prepared sponge color, wherein, in step (3) the binder is an acrylic polymer.

[0032]以上所述的可变色海绵的制备方法,步骤(3)带色抗菌剂溶液和粘结剂重量比例为1:5。 [0032] The method described above may be prepared sponge color, step (3) colored antimicrobial agent solution and the binder weight ratio of 1: 5.

[0033] 实施例3 [0033] Example 3

[0034]取实施例1和实施例2制备得到的可变色海绵进行抗菌实验,结果表明。 [0034] Example 1 taken antibacterial test and discolored sponge prepared in Example 2 obtained results show. 连续使用60天具有很好的抗金黄色葡萄球菌和大肠杆菌的功效,抗菌率95%以上。 60 days of continuous use with good efficacy against Staphylococcus aureus and Escherichia coli, the antibacterial rate of 95% or more.

[0035]以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。 [0035] The above are only preferred embodiments of the present invention, it should be noted that those of ordinary skill in the art, in the present invention without departing from the principles of the premise, can make various improvements and modifications, such modifications and modifications should also be regarded as the protection scope of the present invention.

Claims (7)

1.一种可变色抗菌海绵的制备方法,其特征在于,包括以下步骤: (1)取无色抗菌剂、颜料用溶剂A溶解稀释,在氮封的条件下,升温温到40〜75°C,调节PH值,缓慢滴加耦合剂,控制反应温度,滴加结束后保温2〜5小时,取反应物,静置不分层,再用溶剂A稀释无沉淀物; (2)取步骤(I)溶液加热并恒温到70〜90°C,缓慢滴加缓释型固色剂,控制回流反应速度,避免突沸冲料,滴加结束后,在无回流情况下,继续保温2〜5小时,调节PH值,取回流反应产物,静置不分层,用溶剂A稀释无沉淀物; (3)取步骤(2)带色抗菌剂溶液和粘结剂按比例混合均匀,增稠后用彩色海绵浸渍烘干制成可变色的抗菌海绵。 1. A method of preparing an antimicrobial sponge color, characterized by comprising the steps of: (1) Take a colorless antibacterial agent, a pigment is dissolved diluted with a solvent A, at a nitrogen blanket, and heated to a temperature of 40~75 ° C, adjusting the PH value of the coupling agent was slowly added dropwise, controlling the reaction temperature, holding the end of 2 ~ 5 hours after the dropwise addition, the reaction was taken, allowed to stand without stratification, and then diluted with a solvent A precipitate; (2) from step (I) and the temperature was heated to 70~90 ° C, was slowly added dropwise release fixative, control the reaction rate at reflux, to avoid bumping red material, after the completion of the dropping, in the absence of reflux, incubation was continued for 2 ~ 5 hours, adjusting the PH value, retrieves the reaction product stream, non-hierarchical standing, no precipitate was diluted with a solvent A; (3) from step (2) colored antimicrobial agent and a binder solution was mixed uniformly thickened after drying can be made in color discoloration antimicrobial sponge impregnated sponge.
2.根据权利要求1所述的可变色海绵的制备方法,其特征在于,步骤(I)所述的抗菌剂为有机抗菌剂,颜料为有机颜料,溶剂A为能和醇、酮类溶剂及树脂类粘结剂互溶的有机溶剂。 The preparation method of the color sponge claim 1, wherein step (I) of the antibacterial agent is an organic antimicrobial agent, the pigment is an organic pigment, and an alcohol solvent A was capable, and ketone solvents the binder resin miscible organic solvent.
3.根据权利要求1或2所述的可变色海绵的制备方法,其特征在于,步骤(I)调节PH值7〜10,反应温度为40〜75°C。 The discoloration can be prepared sponge according to claim 1 or 2, wherein the step (I) adjusting the PH value of 7 to 10, the reaction temperature is 40~75 ° C.
4.根据权利要求3所述的可变色海绵的制备方法,其特征在于,步骤(2)所述的固色剂为改性丙烯酸酯类聚合物。 The preparation method of the color sponge claimed in claim 3, wherein the step of fixing agent (2) according to a modified acrylic polymer. 调节PH值为7〜10。 Adjusting the PH value of 7 to 10.
5.根据权利要求1所述的可变色海绵的制备方法,其特征在于,步骤(3)带色抗菌剂为有机抗菌剂,粘结剂为改性丙烯酸酯类聚合物。 The preparation method of the color sponge claim 1, wherein the step (3) the antimicrobial agent is colored organic antimicrobial agent, the binder is a modified acrylic polymer.
6.根据权利要求5所述的可变色海绵的制备方法,其特征在于,步骤(3)带色抗菌剂溶液和粘结剂的重量比为:0.5〜5: 5〜20。 May be discolored sponge preparation process according to claim 5, wherein, in step (3) colored antimicrobial solution and a weight ratio of binder: 0.5~5: 5~20.
7.根据权利要求1所述的可变色海绵的制备方法,其特征在于,步骤(3)耦合剂为硅烷耦合剂。 The preparation method of the color sponge claim 1, wherein the step (3) the coupling agent is a silane coupling agent.
CN201610706013.XA 2016-08-22 2016-08-22 A kind of preparation method of changeable colour antibacterial sponge CN106317448B (en)

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US4311479A (en) * 1977-09-27 1982-01-19 Exterma-Germ Products Ltd. Method of indicating the presence of an impregnant in a substrate
US4678704A (en) * 1985-07-24 1987-07-07 Fibre Treatments (Holding) Limited Impregnated substrate incorporating an indicator dye
US5928665A (en) * 1997-01-29 1999-07-27 Xomed Surgical Products, Inc. Wound dressing including polyvinyl acetal sponge material
CN1934295A (en) * 2004-03-22 2007-03-21 因温斯特技术公司 Low wick continuous filament polyester yarn
CN101896209A (en) * 2007-12-13 2010-11-24 金伯利-克拉克环球有限公司 Self-indicating wipe for removing bacteria from a surface

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4311479A (en) * 1977-09-27 1982-01-19 Exterma-Germ Products Ltd. Method of indicating the presence of an impregnant in a substrate
US4678704A (en) * 1985-07-24 1987-07-07 Fibre Treatments (Holding) Limited Impregnated substrate incorporating an indicator dye
US5928665A (en) * 1997-01-29 1999-07-27 Xomed Surgical Products, Inc. Wound dressing including polyvinyl acetal sponge material
CN1934295A (en) * 2004-03-22 2007-03-21 因温斯特技术公司 Low wick continuous filament polyester yarn
CN101896209A (en) * 2007-12-13 2010-11-24 金伯利-克拉克环球有限公司 Self-indicating wipe for removing bacteria from a surface

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