CN111733021B - Sterilizing washing powder containing PCMX and preparation method thereof - Google Patents

Sterilizing washing powder containing PCMX and preparation method thereof Download PDF

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CN111733021B
CN111733021B CN202010649340.2A CN202010649340A CN111733021B CN 111733021 B CN111733021 B CN 111733021B CN 202010649340 A CN202010649340 A CN 202010649340A CN 111733021 B CN111733021 B CN 111733021B
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antibacterial agent
pcmx
zinc
polyethylene glycol
salt polymer
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CN111733021A (en
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张庆利
杨艳
叶霞
薛念刚
高义祥
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Qingdao Best New Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/83Mixtures of non-ionic with anionic compounds
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/30Biocides, 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
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N31/00Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
    • A01N31/02Acyclic compounds
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N31/00Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
    • A01N31/08Oxygen or sulfur directly attached to an aromatic ring system
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, 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
    • A01N47/40Biocides, 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
    • A01N47/42Biocides, 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
    • A01N47/44Guanidine; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06Powder; Flakes; Free-flowing mixtures; Sheets
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2075Carboxylic acids-salts thereof
    • C11D3/2086Hydroxy carboxylic acids-salts thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/22Carbohydrates or derivatives thereof
    • C11D3/222Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
    • C11D3/225Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin etherified, e.g. CMC
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/48Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/22Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/662Carbohydrates or derivatives

Abstract

The invention provides a PCMX-containing sterilizing washing powder and a preparation method thereof, belonging to the technical field of antibiosis. The sterilizing washing powder containing PCMX is prepared by the following method: s01, preparing the guanidine salt polymer and the polyethylene glycol into the composite antibacterial agent by a physical mixing method according to the proportion; s02, mixing the guanidine salt polymer/polyethylene glycol antibacterial agent with a zinc-carrying antibacterial agent, Parachlorometaxylenol (PCMX) and dioctyl sodium sulfosuccinate to prepare the PCMX-containing composite antibacterial agent, wherein the composite antibacterial agent can be added into washing powder, soap powder and other washing formula systems, is quickly dissolved and dispersed when clothes are washed, releases guanidine salt polymer, zinc ions and parachlorometaxylenol antibacterial components, and has the functions of quick sterilization and degerming.

Description

Sterilizing washing powder containing PCMX and preparation method thereof
Technical Field
The invention relates to the technical field of antibiosis, in particular to sterilizing washing powder containing PCMX and a preparation method thereof, wherein the washing powder can be quickly dissolved in water and has the functions of sterilization and degerming.
Background
In recent years, with the increasing economic level of people, the requirement for sanitation in life is higher, and a certain amount of disinfectant is often added by consumers when clothes are washed. Common disinfectant in the market generally contains effective components such as sodium hypochlorite, hydrogen peroxide, but sodium hypochlorite, hydrogen peroxide etc. have strong oxidizing property, probably can cause the clothing to fade, if remain on the clothes, cause irritative pruritus to skin, easily cause the damage to domestic non professional washing personnel. Therefore, it is very necessary to develop a milder, highly efficient and broad-spectrum antibacterial compound for washing.
The guanidine salt polymer (polyguanidine) is a polymer based on a guanidine group, has the excellent performances of high safety, broad sterilization spectrum, low effective concentration, high action speed, stable property, easy water dissolution and the like, is harmless to human body temperature, is an environment-friendly antibacterial agent, and has extremely wide application in industry, agriculture, medical use and daily life. The currently available types of guanidine salt polymers include polyhexamethylene (bis) guanidine hydrochloride, polyhexamethylene (bis) guanidine propionate, polyhexamethylene (bis) guanidine stearate, or other inorganic and organic acid salts of polyhexamethylene (bis) guanidine, polyoxyethylene guanidine, etc., and many new guanidine salt polymers are being developed.
Parachlorometaxylenol (PCMX) is a broad-spectrum antibacterial agent, has the effect of killing most gram-positive and gram-negative bacteria, fungi and molds, and can be widely applied to disinfection or personal care products as a mildew-proof antibacterial agent, such as antibacterial detergents of anti-dandruff shampoos, hand washing liquids, soaps, other sanitary products and the like. The parachlorometaxylenol has low solubility in water and is easily dissolved in solvents such as alcohol, ether, polyglycol and the like. In order to better exert the function of parachlorometaxylenol, polyethylene glycol is introduced into a formula system, and parachlorometaxylenol powder with smaller particle size is used, so that the parachlorometaxylenol powder is easier to disperse during washing.
According to a large number of formula tests, by optimizing a surfactant system, compounding various antibacterial agents and other methods, the invention provides the sterilizing washing powder containing PCMX and the preparation method thereof, the sterilizing washing powder with antibacterial agents such as guanidine salt polymer and parachlorometaxylenol as main components is prepared, the uniformity is good, the use is convenient, the parachlorometaxylenol is compounded with the guanidine salt polymer, the broad spectrum and the high efficiency of sterilization during washing are improved, the guanidine salt polymer, the zinc ion antibacterial agent, the parachlorometaxylenol and other components can be quickly released during washing, and the effects of sterilization and degerming are achieved.
Disclosure of Invention
The invention provides a sterilizing washing powder containing PCMX and a preparation method thereof, wherein the active ingredients are guanidine salt polymer/polyethylene glycol/zinc-loaded antibacterial agent/parachlorometaxylenol/dioctyl sodium sulfosuccinate, and the sterilizing washing powder can be added into a washing powder, soap powder and other formula systems, can be quickly dissolved in the washing process, fully acts with fabrics, and has the effects of sterilization and degerming.
The sterilizing washing powder containing PCMX is prepared by the following method:
s01, preparing a guanidine salt polymer/polyethylene glycol composite antibacterial agent, and preparing the guanidine salt polymer/polyethylene glycol composite antibacterial agent by physically mixing the guanidine salt polymer and polyethylene glycol according to a proportion, wherein the weight ratio of the guanidine salt polymer to the polyethylene glycol is 90: 10-99: 1, and the preferable weight ratio is 95: 5-99: 1; the polyethylene glycol contains a large amount of hydroxyl groups, has good water solubility, is preferably polyethylene glycol with the molecular weight of 600-2000, is slow in water solubility when the molecular weight is too large, is relatively poor in compatibility with a guanidinium polymer, can be fully mixed with molecular chains of the polyethylene glycol after being fully physically mixed with the guanidinium polymer, increases the instant solubility of the guanidinium polymer, can be more fully used with clothing fibers, and plays a better sterilization effect, and in addition, the sterilization efficiency is obviously improved after the polyethylene glycol is introduced;
s02: preparing a PCMX-containing composite antibacterial agent, mixing a guanidine salt polymer/polyethylene glycol composite antibacterial agent with a zinc-carrying antibacterial agent, Parachlorometaxylenol (PCMX) and dioctyl sodium sulfosuccinate, and physically mixing by a stirrer and the like to prepare the PCMX-containing composite antibacterial agent, wherein the weight ratio of the zinc-carrying antibacterial agent to the parachlorometaxylenol is preferably 50: 50-70: 30; the weight sum of the zinc-loaded antibacterial agent and the parachlorometaxylenol and the preferable weight sum of the dioctyl sodium sulfosuccinate are 70: 30-90: 10; wherein the total weight ratio of the guanidine salt polymer/polyethylene glycol composite antibacterial agent to the zinc-carrying antibacterial agent, the parachlorometaxylenol and the dioctyl sodium sulfosuccinate is 50: 50-95: 5, and the preferable weight ratio is 60: 40-90: 10; by optimizing the proportion of guanidine salt polymer, polyethylene glycol, zinc ion antibacterial agent, parachlorometaxylenol and dioctyl sodium sulfosuccinate and fully and uniformly stirring the components, the composite antibacterial agent with good uniform hydrophilicity can be formed; the guanidine salt polymer/polyethylene glycol composite antibacterial agent is compounded with the zinc ion antibacterial agent, and the zinc ion antibacterial agent with the inorganic carrier is introduced, so that the zinc ion and the guanidine salt polymer can be compounded, and the antibacterial effect is further improved; the guanidine salt polymer/polyethylene glycol composite antibacterial agent is compounded with the zinc ion antibacterial agent and the chloroxylenol, so that the antibacterial effect is further improved, the antifungal effect is particularly high, and the sterilization efficiency and the broad spectrum are improved; the dioctyl sodium sulfosuccinate can effectively improve the hydrophilicity and the wettability of the whole antibacterial system, so that the dioctyl sodium sulfosuccinate can play a role more efficiently during washing.
Further, the temperature of the guanidine salt polymer, the polyethylene glycol, the zinc-loaded antibacterial agent, the parachlorometaxylenol and the dioctyl sodium sulfosuccinate when mixed according to the proportion is not more than 40 ℃.
Further, S03: preparing sterilizing washing powder containing PCMX, compounding a compound antibacterial agent containing PCMX with a surfactant, coconut oil fatty diethanolamide, lauryl glucoside, sodium citrate, water and sodium carboxymethylcellulose, and fully and uniformly mixing in a low-speed mixer to prepare the powdery sterilizing washing powder, wherein the mixture ratio of the components is as follows (weight percentage):
PCMX-containing complex antimicrobial agents: 0.5 to 5 percent
Surfactant (b): 3 to 5 percent
Coconut oil fatty diethanolamide: 24 to 50 percent
Lauryl glucoside: 10 to 30 percent
Sodium citrate: 1 to 3 percent
Water: 15 to 30 percent
Sodium carboxymethylcellulose: 1 to 3 percent.
Further, the guanidine salt polymer is at least one of polyhexamethylene guanidine hydrochloride, polyhexamethylene biguanide hydrochloride, polyhexamethylene guanidine nitrate, polyhexamethylene biguanide nitrate, polyhexamethylene guanidine carbonate, polyhexamethylene biguanide carbonate, polyhexamethylene guanidine propionate, polyhexamethylene biguanide propionate, polyhexamethylene guanidine phosphate and polyhexamethylene biguanide phosphate.
Furthermore, the zinc ion antibacterial agent is an antibacterial agent with zinc ions as a main antibacterial component, the carrier is 4A zeolite, 5A zeolite, natural zeolite, diatomite, montmorillonite and kaolin, the content of the zinc ions is 10-50 wt%, the 4A zeolite is preferred, the content of the zinc ions is preferably 20-30 wt%, the proportion of the zinc ion antibacterial agent is too high, or the content of the zinc ions in the antibacterial agent is too high, so that the dissolved zinc ions are too fast, a complex compound can be formed with a guanidinium polymer, the activity of the molecular chain movement of the guanidinium polymer is reduced, the content of the zinc ion antibacterial agent is too low, or the content of the zinc ions in the antibacterial agent is too low, so that the antibacterial efficiency is too low. The zeolite-carried zinc has better effect and is possibly related to the cubic form, hardness, particle size and the like of the zeolite, and inorganic carriers such as the zeolite and the like can generate friction with fabrics in the washing process, so that the molecular chain of the guanidine salt polymer is driven to act on the fabrics, and the antibacterial effect is further improved.
Further, the particle diameter D90 of the parachlorometaxylenol is preferably 300nm to 2 μm, and preferably 300nm to 1 μm.
Furthermore, the molecular weight of the polyethylene glycol is 600-20000, preferably 600-2000.
Further, the surfactant is at least one of sodium dodecyl benzene sulfonate, sodium lauryl sulfate and fatty alcohol-polyoxyethylene ether sodium sulfate.
The invention also provides a preparation method of the sterilizing washing powder containing PCMX, which comprises the steps of uniformly mixing the PCMX-containing composite antibacterial agent, the surfactant, the coconut oil fatty diethanolamide, the lauryl glucoside, the sodium citrate, the water and the sodium carboxymethyl cellulose according to the sequence and the content, and fully and uniformly mixing in a low-speed mixer to prepare the powdery sterilizing washing powder.
The invention also provides the application of the PCMX-containing sterilizing washing powder prepared by the preparation method, and the PCMX-containing sterilizing washing powder is quickly dissolved and dispersed when clothes are washed, and releases guanidine salt polymer, zinc ions and parachlorometaxylenol components to play a role in quick sterilization.
The invention provides a sterilizing washing powder containing PCMX and a preparation method thereof, which comprises active ingredients such as guanidine salt polymer/polyethylene glycol/zinc-loaded antibacterial agent/p-chloroxylenol/dioctyl sodium sulfosuccinate and the like, can be added into formula systems such as laundry clothes, soap powder and the like, can quickly and continuously release antibacterial components such as guanidine salt polymer, zinc ions, p-chloroxylenol and the like during washing, has the functions of quick sterilization and degerming, enables clothes to be cleaner and more sanitary, and has the advantages of high safety, convenience in use and high efficiency of degerming.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic representation of a powdered complex antimicrobial agent comprising PCMX prepared according to the present invention.
FIG. 2 is a schematic diagram of the sterilizing washing powder containing PCMX prepared by the invention.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer and more complete description of the present invention will be given below with reference to specific embodiments, and it is obvious that the described embodiments are some but not all embodiments of the present invention, and all other embodiments obtained by a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
The raw materials and equipment involved in the embodiment of the invention are as follows:
polyhexamethylene guanidine hydrochloride: hubeidingchengjingshikai pharmaceutical chemical Co., Ltd, CAS No.57028-96-3, powder;
zinc-loaded antimicrobial agents: zinc content 30%, Z301, powder, commercially available;
polyethylene glycol: the molecular weight is 600-2000, the chemical purity is high, and the molecular weight is commercially available;
p-chloro-m-xylenol: d90<2 μm, commercially available;
sodium dioctyl sulfosuccinate: AEROSOLOT100, Cyanid Inc.;
sodium dodecylbenzenesulfonate: chemically pure, commercially available;
coconut oil fatty diethanolamide: is sold on the market;
lauryl glucoside: is sold on the market;
sodium citrate: chemically pure, commercially available;
sodium carboxymethylcellulose: fushan Ri Special chemical Co., Ltd, commercially available;
preparation of PCMX-containing composite antibacterial agent
1. Preparation of guanidine salt polymer/polyethylene glycol composite antibacterial agent
The water-soluble polyhexamethylene guanidine hydrochloride and polyethylene glycol (different molecular weights) are uniformly stirred in a stirrer according to the proportion shown in the table 1 to prepare the guanidine salt polymer/polyethylene glycol composite antibacterial agent.
Table 1.
Figure BDA0002574311400000061
Figure BDA0002574311400000071
2. Preparation of compound antibacterial agent containing PCMX
2.1 preparation of Zinc-loaded antimicrobial agent/p-chloro-m-xylenol
The zinc-carrying antibacterial agent and the parachlorometaxylenol are mixed according to the proportion shown in the table 2 and are stirred uniformly.
Table 2.
Numbering Zinc-loaded antimicrobial agent/g Parachlorometaxylenol/g
Comparative example 17 450 550
Example 10 500 500
Example 11 600 400
Example 12 700 300
Comparative example 18 750 250
Comparative example 19 1000 0
2.2 preparation of Zinc-loaded antibacterial agent/P-chloro-m-xylenol/sodium dioctyl sulfosuccinate composite antibacterial agent
The zinc-carrying antibacterial agent/p-chloro-m-xylenol and sodium dioctyl sulfosuccinate are mixed according to the proportion shown in the table 3 and stirred uniformly.
Table 3.
Numbering Zinc-loaded antibacterial agent/p-chloro-m-xylenol/g Dioctyl succinate sodium sulfonate/g
Comparative example 20 Example 11/750 250
Example 13 Example 11/700 300
Examples14 Example 11/800 200
Example 15 Example 11/900 100
Comparative example 21 Example 11/950 50
Comparative example 22 Example 11/1000 0
Comparative example 23 Comparative example 19/800 200
2.3 preparation of a Compound antibacterial agent containing PCMX
The prepared water-soluble polyhexamethylene guanidine hydrochloride and polyethylene glycol are uniformly stirred in a stirrer, then the zinc-loaded antibacterial agent, parachlorometaxylenol and dioctyl sodium sulfosuccinate shown in the table 4 are added and continuously stirred uniformly, and the powdery compound antibacterial agent containing PCMX (shown in figure 1) is prepared by a physical mixing method such as a stirrer and the like.
Table 4.
Numbering Guanidine salt polymer/polyethylene glycol/g Zinc-loaded antibacterial agent/parachlorometaxylenol/dioctyl sodium sulfosuccinate/g
Comparative example 24 Comparative example 12/850 Example 14/150
Comparative example 25 Example 5/450 Example 14/550
Example 16 Example 5/500 Example 14/500
Example 17 Example 5/600 Example 14/400
Example 18 Example 5/700 Example 14/300
Example 19 Example 5/800 Example 14/200
Example 20 Example 5/900 Example 14/100
Example 21 Example 5/950 Example 14/50
Comparative example 26 Example 5/970 Example 14/30
Comparative example 27 Example 5/700 Comparative example 22/300
Comparative example 28 Example 5/700 Comparative example 23/300
Secondly, preparation of sterilizing washing powder containing PCMX
The prepared PCMX-containing composite antibacterial agent is mixed with water, sodium dodecyl benzene sulfonate, coconut oil fatty diethanolamide, lauryl glucoside, sodium citrate and sodium carboxymethylcellulose according to the proportion designed in the table 5 in a low-speed stirrer to prepare the PCMX-containing sterilizing washing powder (shown in figure 2) with good component dispersibility, high sterilizing efficiency and uniformity.
Table 5.
Figure BDA0002574311400000081
Figure BDA0002574311400000091
Thirdly, evaluating the sterilization effect of the sterilizing washing powder containing PCMX in water
The PCMX-containing disinfecting washing powder prepared in any one of comparative example 29, comparative example 30, comparative example 31 and examples 22-42 and used in the example 29 for evaluating the disinfecting effect when washing clothes. Referring to the sterilization detection method of GB21551.5-2010 antibacterial, sterilization and purification functions of household and similar electric appliances-Special requirements of washing machines, standard washing materials are added into a common 10 kg washing machine without sterilization function: the bleaching medium plain cloth required by GB/T411 is characterized in that a kerchief of 330mm x 330mm is prepared by desizing treatment of 21 +/-2 counts of warp yarns and 21 +/-2 counts of weft yarns. Test sample cloth: the bleaching medium plain cloth required by GB/T411 is characterized in that 21 +/-2 counts of warp yarns and 21 +/-2 counts of weft yarns are subjected to desizing treatment to prepare square cloth with the thickness of 100mm multiplied by 100mm, and the total weight is 3 kilograms.
Uniformly coating 1mL of a diluted solution of a bacterial solution on each test sample block cloth with the size of 100mm multiplied by 100mm, preparing 2 washing machines with the same model according to an operation method disclosed in appendix A in GB21551.5, adding the sterilizing washing powder into one washing machine, not adding the sterilizing washing powder into the other washing machine (reference sample), starting a washing program, taking out the test cloth after the washing program is finished, and testing the number of the residual viable bacteria on the test sample blocks by adopting a viable bacteria counting method. And (3) detecting bacteria: staphylococcus aureus, Escherichia coli, Candida albicans, and bacterial liquid concentration of 1.0 × 109~9.0×109CFU/mL. The experiment was repeated 3 times, and the respective sterilization rates were calculated, and the average values were taken, and the addition amounts and sterilization effects of the sterilization detergent powders are shown in table 7.
The calculation formula is as follows:
Figure BDA0002574311400000101
table 7.
Figure BDA0002574311400000102
After meeting water, the sterilizing washing powder containing PCMX can quickly and continuously release guanidine salt polymer, zinc ions, parachlorometaxylenol and other components, and is added when clothes are washed, so that the functions of quick sterilization and sterilization are achieved. The sterilizing effect is shown in table 7, when the addition amount of the sterilizing washing powder is more than 5g, the sterilizing rate of escherichia coli, staphylococcus aureus and candida albicans is as high as 99.9%, and a good antibacterial effect can be achieved, when the addition amount of the sterilizing washing powder is far more than 5g, the antibacterial effect achieved is basically the same as that achieved when the addition amount is slightly more than 5g, but in specific application, the dosage can be adjusted according to the degree of pollution of the washing clothes, the types of bacterial pollution are different, the dosage can be properly increased, for example, the dosage of the hospital-polluted clothes and the like, and the capacities, the rotating speeds and the powers of different washing machines are different, and the dosage of the sterilizing washing powder is also different. In the embodiment, when clothes are washed, the addition amount of the sterilizing washing powder is between 5g and 10g, so that the antibacterial washing powder not only has a good antibacterial effect, but also can effectively save resources. According to the preparation of the guanidine salt polymer/polyethylene glycol composite antibacterial agent, polyethylene glycol contains a large number of hydroxyl groups, the polyethylene glycol has good water solubility, the polyethylene glycol with the molecular weight of 600-2000 is preferable, the polyethylene glycol with the molecular weight of 60000 has low dissolution speed, and the antibacterial washing powder prepared by the polyethylene glycol with the molecular weight of 60000 has undissolved solid particles after being washed by a washing machine of comparative example 29, so that the antibacterial rate is low.
The guanidine salt polymer/polyethylene glycol/zinc-loaded antibacterial agent/p-chloroxylenol/dioctyl sodium sulfosuccinate is prepared, the proportion of the zinc-loaded antibacterial agent in the comparative example 18 is too large, when the zinc-loaded antibacterial agent is uniformly stirred, the formed composite antibacterial agent has poor hydrophilicity, insoluble particle residues are easy to exist after washing, and the sterilization effect after washing in the comparative example 34 shows that the sterilization rate of candida albicans (fungi) added with the p-chloroxylenol in the composite antibacterial agent is obviously superior to that of the composite antibacterial agent without the p-chloroxylenol. In comparative example 33, the degerming detergent powder without adding dioctyl sodium sulfosuccinate was added after the washing machine was started, and after a short time of washing for 20 minutes, the residual granular substance, which may be parachlorometaxylenol with poor hydrophilicity, was found on the clothes after washing, causing insoluble components to agglomerate, and the washing time was short, and the agglomerate remained on the surface of the clothes fiber, easily causing the contamination of the clothes. Meanwhile, the antibacterial rate of Candida albicans (fungi) is obviously better than that of the added sodium dioctyl sulfosuccinate. It follows that the weight ratio of zinc-loaded antimicrobial agent to parachlorometaxylenol is preferably 50: 50-70: 30; the weight sum of the zinc-loaded antibacterial agent and the parachlorometaxylenol and the preferable weight sum of the dioctyl sodium sulfosuccinate are 70: 30-90: 10; wherein the total weight ratio of the guanidine salt polymer/polyethylene glycol composite antibacterial agent to the zinc-carrying antibacterial agent, the parachlorometaxylenol and the dioctyl sodium sulfosuccinate is 50: 50-95: 5, and the preferable weight ratio is 60: 40-90: 10.
In summary, the embodiments of the present invention can at least achieve the following beneficial effects:
1. the invention provides a compound antibacterial agent containing PCMX, which is added into washing formulas of washing powder or soap powder and the like, and 5-10 g of the compound antibacterial agent is added during washing of a washing machine, can be quickly dissolved and has the functions of removing and killing pathogenic microorganisms such as bacteria, fungi and the like.
2. By compounding the guanidine salt polymer and the polyethylene glycol, the dissolving speed of the polyguanidine antibacterial agent added into water is improved, the polyguanidine antibacterial agent is compatible with fabrics and other detergents, and the permeability of the polyguanidine antibacterial agent to the fabrics is improved, so that a better antibacterial effect is achieved.
3. By compounding the guanidine salt polymer with the zinc-loaded antibacterial agent, the parachlorometaxylenol and the dioctyl sodium sulfosuccinate, the broad spectrum and the antibacterial efficiency of the antibacterial are improved, the using amount is reduced, and the time for washing and sterilizing is shortened.
4. Preferably, the zeolite zinc-loaded antibacterial agent and the guanidine salt polymer are compounded, and when the fabric is washed, the water-soluble guanidine salt polymer antibacterial agent and zinc ions are released simultaneously by utilizing the friction between the zeolite and the fabric, and the antibacterial agent and the microorganisms such as bacteria on the surface of the fabric are contacted repeatedly by cooperating with the antibacterial effect, so that a better antibacterial effect is achieved.
5. The parachlorometaxylenol has more efficient fungal effect, and the antibacterial efficiency and broad spectrum are improved; the sodium dioctyl sulfosuccinate can effectively improve the hydrophilicity and wettability of an antibacterial system and increase the sterilization rate of clothes during washing.
Finally, it is to be noted that: the above description is only a preferred embodiment of the present invention, and is only used to illustrate the technical solutions of the present invention, and not to limit the protection scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.

Claims (4)

1. The sterilizing washing powder containing PCMX is characterized by being prepared by the following method:
s01, preparing a guanidine salt polymer/polyethylene glycol composite antibacterial agent, and preparing the guanidine salt polymer/polyethylene glycol composite antibacterial agent by physically mixing the guanidine salt polymer and polyethylene glycol according to a proportion, wherein the weight ratio of the guanidine salt polymer to the polyethylene glycol is 90: 10-99: 1;
s02: preparing a PCMX-containing composite antibacterial agent, and mixing a guanidine salt polymer/polyethylene glycol composite antibacterial agent with a zinc-carrying antibacterial agent, Parachlorometaxylenol (PCMX) and dioctyl sodium sulfosuccinate to prepare the PCMX-containing composite antibacterial agent, wherein the weight ratio of the zinc-carrying antibacterial agent to the parachlorometaxylenol is 50: 50-70: 30; the sum of the weight of the zinc-carrying antibacterial agent and the p-chloro-m-xylenol and the weight of the dioctyl sodium sulfosuccinate are 70: 30-90: 10; wherein the weight ratio of the guanidine salt polymer/polyethylene glycol composite antibacterial agent to the zinc-carrying antibacterial agent to the parachlorometaxylenol and the dioctyl sodium sulfosuccinate is 50: 50-95: 5;
s03: preparing sterilizing washing powder containing PCMX, compounding a compound antibacterial agent containing PCMX with a surfactant, coconut oil fatty diethanolamide, lauryl glucoside, sodium citrate, water and sodium carboxymethylcellulose, and fully and uniformly mixing in a low-speed mixer to prepare the powdery sterilizing washing powder, wherein the mixture ratio of the components is as follows by weight percent:
PCMX-containing complex antimicrobial agents: 0.5 to 5 percent
Surfactant (b): 3 to 5 percent
Coconut oil fatty diethanolamide: 24 to 50 percent
Lauryl glucoside: 10 to 30 percent
Sodium citrate: 1 to 3 percent
Water: 15 to 30 percent
Sodium carboxymethylcellulose: 1-3%;
the surfactant is at least one of sodium dodecyl benzene sulfonate, sodium lauryl sulfate and fatty alcohol-polyoxyethylene ether sodium sulfate;
the molecular weight of the polyethylene glycol is 600-2000;
the zinc-carrying antibacterial agent is an antibacterial agent with zinc ions as a main antibacterial component, the carrier is 4A zeolite, 5A zeolite and natural zeolite, and the zinc ion content is 30% by weight;
the guanidine salt polymer is polyhexamethylene guanidine hydrochloride.
2. The sterilizing detergent powder containing PCMX according to claim 1, wherein the guanidine salt polymer, polyethylene glycol, zinc-loaded antibacterial agent, parachlorometaxylenol, dioctyl sodium sulfosuccinate are mixed in proportion at a temperature not exceeding 40 ℃.
3. The sterilizing washing powder containing PCMX according to claim 2, wherein the parachlorometaxylenol particle size D90 is 300 nm-2 μm.
4. The method for preparing the sterilizing washing powder containing PCMX according to any one of claims 2 to 3, wherein the compound antibacterial agent containing PCMX is uniformly mixed with the surfactant, the coconut oil fatty diethanolamide, the lauryl glucoside, the sodium citrate, the water and the sodium carboxymethyl cellulose according to the sequence and the content in the claim 1, and the mixture is fully and uniformly mixed in a low-speed mixer to prepare the powdery sterilizing washing powder.
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