CN114989905A - Washing gel bead with sterilization and disinfection effects and preparation method thereof - Google Patents

Washing gel bead with sterilization and disinfection effects and preparation method thereof Download PDF

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CN114989905A
CN114989905A CN202210765798.3A CN202210765798A CN114989905A CN 114989905 A CN114989905 A CN 114989905A CN 202210765798 A CN202210765798 A CN 202210765798A CN 114989905 A CN114989905 A CN 114989905A
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bead
effects
sterilization
laundry
germicidal
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CN114989905B (en
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张少雄
汤美娟
黄平
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Guangdong Youkai Technology Co ltd
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    • C11D3/16Organic compounds
    • C11D3/37Polymers
    • C11D3/3703Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • C11D1/02Anionic compounds
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Abstract

The invention relates to a washing condensation bead with sterilization and disinfection effects and a preparation method thereof, wherein the washing condensation bead with sterilization and disinfection effects comprises a content and an outer layer; wherein the content comprises the following components in percentage by mass: 5-30% of parachlorometaxylenol, 2-20% of polyethylene glycol, 18-35% of dodecylbenzene sulfonic acid, 20-40% of other solvents, 5-20% of anionic surfactant, 3-10% of neutralizing agent, 1-20% of nonionic surfactant, 0.1-3% of auxiliary agent and water; the outer layer is a polyvinyl alcohol film. The invention ensures that the product has stronger sterilization and disinfection capability, the prepared washing gel bead has good pressure resistance, the outer layer of the product is stiff and does not collapse, the liquid can be prevented from permeating from a PVA film, and the product has excellent high-low temperature stability and does not precipitate or delaminate under various conditions.

Description

Washing gel bead with sterilization and disinfection effects and preparation method thereof
Technical Field
The invention belongs to the technical field of fabric washing and nursing, and particularly relates to a washing gel bead with a sterilization and disinfection effect and a preparation method thereof.
Background
At present, with consumers focusing on healthy life, daily chemical washing products are required to bring additional value besides meeting daily washing requirements, so that various products are produced, and the daily chemical washing products are developed towards multiple functions, such as functions of softening, sterilizing, color protecting and the like, but most products are only concept declarations and cannot achieve additional effects well.
Therefore, the development of the washing gel bead product which can efficiently sterilize and disinfect while washing and decontaminating, can be quantitatively and conveniently used so as to meet the requirements of consumption and healthy life has important significance and wide market prospect.
There are currently laundry bead products that incorporate bactericides into compositions, such as: a laundry bead product that employs a mixture of N, N-didecyl-N, N-dimethylammonium chloride (2280) bactericide and dodecyl dimethyl benzyl ammonium chloride (1227), polyhexamethylene biguanide hydrochloride (IB), didecyl methyl hydroxyethyl ammonium chloride (DEQ) cationic surfactant; the product with improved sterilizing effect is realized by using the silver ion bactericide; the efficient sterilization washing coagulated bead product is realized by compounding triclosan and PCMX (parachlorometaxylenol) bactericide.
However, the technical scheme does not solve the problems that the oil-soluble bactericide is insoluble in water, and is easy to disperse unevenly in the product and generate precipitates when being matched with a common solvent, and the problem that the stability of the product is insufficient because the outer layer of the beading is easy to collapse and break due to the change of the adding amount of the common solvent.
In summary, there is a need to develop a new technical solution to provide a more stable washing gel bead product with sterilization and disinfection effects to solve the problems existing in the prior art and meet the development requirements of the current market.
Disclosure of Invention
Based on the above, the invention develops a washing gel bead with sterilization and disinfection effects to overcome the defects of the prior art. The invention adopts the reasonable proportion of the polyethylene glycol solvent and other solvents, and is compounded with the dodecylbenzene sulfonic acid surfactant, so that a large amount of PCMX can be fully dissolved in a formula system, the product has stronger sterilization and disinfection capacity, the prepared laundry gel bead has good compression resistance, the outer layer of the product is stiff and not soft, the liquid can be prevented from permeating from a PVA film, and the product has excellent high and low temperature stability, and does not precipitate or delaminate under various conditions.
One object of the present invention is to provide a washing bead with sterilization and disinfection effects, which comprises a content and an outer layer;
wherein the content of the first and second substances,
the content comprises the following components in percentage by mass:
Figure BDA0003725507490000021
the outer layer of the washing condensation bead with the sterilization and disinfection effects is a polyvinyl alcohol film;
wherein the content of the first and second substances,
the polyethylene glycol has the following structural general formula:
Figure BDA0003725507490000022
wherein n is 2 to 8.
Further, the content comprises the following components in percentage by mass:
Figure BDA0003725507490000023
further, the molecular weight of the polyethylene glycol is 100-400.
Further, the mass ratio of the polyethylene glycol to other solvents is not less than 1: 4.
Further, the mass ratio of the polyethylene glycol to other solvents is not less than 1: 3.
Further, the thickness of the polyvinyl alcohol film is 30-120 μm.
Further, the thickness of the polyvinyl alcohol film is preferably 70 to 100. mu.m.
Further, the appearance form of the washing condensation bead with the sterilization and disinfection effect is selected from one of a single cavity, a double cavity and a three cavity.
Further, the other solvent is selected from one or more of glycerol, 1, 2-propylene glycol, isopropanol and ethanol.
Further, the anionic surfactant is selected from one or more of sodium fatty alcohol polyoxyethylene sulfate, oleic acid, lauric acid and coconut oil acid.
Further, the neutralizing agent is selected from one or more of sodium hydroxide, potassium hydroxide, monoethanolamine, diethanolamine, triethanolamine.
Further, the nonionic surfactant is selected from one or more of fatty alcohol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether, isomeric decyl alcohol polyoxyethylene ether and fatty acid methyl ester ethoxylate.
Further, the auxiliary agent is selected from one or more of fluorescent whitening agent, enzyme preparation, anti-redeposition agent, essence and pigment.
Further, the essence is selected from perfume ingredients suitable for daily chemical washing products, and the pigment is selected from dyes and pigments suitable for cosmetics.
Another object of the present invention is to provide a method for preparing the above laundry beads with sterilization and disinfection effects, wherein the method for preparing the laundry beads with sterilization and disinfection effects comprises the following steps:
s1, adding parachlorometaxylenol into a mixed solution of polyethylene glycol and other solvents, and stirring for dissolving;
s2, sequentially adding a neutralizing agent and dodecyl benzene sulfonic acid, stirring and dissolving, and then raising the temperature of the solution;
s3, adding an anionic surfactant, stirring for reaction, then adding a nonionic surfactant, and stirring until the mixture is clear and transparent;
s4, cooling, adding an auxiliary agent and water, and uniformly stirring to obtain a concentrated solution;
and S5, sealing and packaging the concentrated solution by using a polyvinyl alcohol film to obtain the washing gel bead with the sterilization and disinfection effects.
The invention has the following beneficial effects:
1. the washing gel bead with the sterilization and disinfection effects has good sterilization and disinfection capability, and the sterilization effect on staphylococcus aureus, escherichia coli, klebsiella pneumoniae and candida albicans is as high as 99.9 percent
2. The polyethylene glycol and other solvents are compounded in a certain proportion, and the finding that the PCMX can be well dissolved and the PVA-coated coagulated beads can be kept rigid and not collapsed is unexpected. The polyethylene glycol has a certain number of ether groups and two hydroxyl groups, so that the polyethylene glycol has better solubility; the number of carbon atoms of the hydrophobic chain segment is more than that of other solvents, and the hydrophobic chain segment is used as a hydrophobic chain segment to better prevent hydroxyl of the solvent from permeating the PVA polyvinyl alcohol water-soluble film, so that the condensed beads are prevented from soft collapse. In addition, the dodecyl benzene sulfonic acid is compounded with the polyethylene glycol in a certain proportion, so that the stiffness of the coagulated beads can be further improved. Through analysis, the sulfonic acid group of the dodecylbenzene sulfonic acid is not strong in hydrophilicity, but the benzene ring contained in the dodecylbenzene sulfonic acid has certain steric hindrance effect, so that other surface active and solvent can be better solubilized, and the hydrophilic group is prevented from being excessively permeated into a PVA water-soluble film, so that the outer layer of the condensed bead is prevented from generating soft collapse. The two components are compounded according to a specific proportion, so that a good synergistic effect is achieved, the prepared coagulated beads have good pressure resistance, the liquid in a PVA film can be prevented from permeating, the plumpness and the stiffness of the outer layer of the coagulated beads are kept, and the effect cannot be achieved by adding a single component.
3. The washing gel bead with the sterilization and disinfection effects has good stability, can keep no layering and no precipitation in low-temperature, high-temperature or high-humidity environments, ensures the use experience and performance of products, and has good application prospect.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following examples are given. The starting materials, reactions and work-up procedures which are given in the examples are, unless otherwise stated, those which are customary on the market and are known to the person skilled in the art.
The words "preferred", "preferably", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
It should be understood that other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention.
Glycerol in the examples of the present invention: solvent, purchased from Lithocarpus tikoua brown.
1, 2-propanediol in the examples of the present invention: solvent, available from SK, korea.
Polyethylene glycol 1(n ═ 2) in the examples of the present invention: purchased from Guangzhou reagent works.
Polyethylene glycol 2(n ═ 4) in the examples of the present invention: molecular weight 200, available from Guangzhou reagent works.
Isopropyl alcohol in the examples of the present invention: solvent, available from Guangzhou Kaihong chemical Co.
PCMX in the examples of the present invention: p-chloro-m-xylenol available from Netchem Inc Canada.
Monoethanolamine in the examples of the present invention: neutralizer, available from basf.
Triethanolamine in the examples of the invention: neutralizer, available from basf.
Dodecyl sulfonic acid in the examples of the present invention: anionic surfactant, purchased from south beautiful ministers of lake.
Oleic acid in the examples of the present invention: anionic surfactants, available from pacific oil.
AES in the embodiment of the present invention: anionic surfactants, available from zahn science.
AEO9 in the present embodiment: nonionic surfactant, available from basf.
TO8 in the present example: isomeric tridecanol polyoxyethylene ethers, nonionic surfactants, available from the Pasteur Lutensol series list.
MEE in the embodiment of the invention: nonionic surfactant, available from LION, Japan.
The respective components and the respective parts by mass of the laundry beads having sterilizing and disinfecting effects of examples 1 to 3 and the laundry beads of comparative examples 1 to 4 are shown in table 1.
TABLE 1 Components and their mass fractions (contents) in examples 1 to 3 and comparative examples 1 to 4
Figure BDA0003725507490000051
Examples 1-3 methods for preparing laundry beads with germicidal and disinfectant effects were all as follows:
s1, adding PCMX into a mixed solution of polyethylene glycol and other solvents according to the mass fraction, and stirring and dissolving;
s2, sequentially adding a neutralizing agent and dodecyl benzene sulfonic acid, stirring for 10min, and raising the temperature of the solution to 50 ℃ after complete dissolution;
s3, adding an anionic surfactant, stirring for reacting for 20min, then adding a nonionic surfactant, and stirring until the mixture is clear and transparent;
s4, cooling to 45 ℃, adding an auxiliary agent and water, and uniformly stirring to obtain a concentrated solution;
and S5, carrying out film sealing and packaging on the concentrated solution in a film sealing and packaging machine by using polyvinyl alcohol to obtain the washing condensation bead with the sterilization and disinfection effects.
The laundry beads of comparative examples 1-4 differ from examples 1-3 in that: the polyethylene glycol component is deleted or replaced, and other preparation methods and steps are the same.
Examples 4-6 and comparative examples 5-6 were additionally set for stability testing, and the individual ingredients and corresponding parts by mass of the laundry beads having sterilizing and disinfecting effects of examples 4-6 and the laundry beads of comparative examples 5-6 are shown in table 2.
TABLE 2 ingredients and their mass fractions in examples 4 to 6 and comparative examples 5 to 6
Example 4 Example 5 Example 6 Comparative example 5 Comparative example 6
Composition comprising a fatty acid ester and a fatty acid ester H I J K L
Components Content (%) Content (%) Content (%) Content (%) Content (%)
Glycerol 10 10 10 20 15
1, 2-propanediol 15 15 15 5 5
PCMX 5 12 15 12 15
Polyethylene glycol 2 8 8 15 5 15
Mono-ethanol amine 4 4 4 3 1
Triethanolamine 1 1 1 1 1
Dodecyl benzene sulfonic acid 22 20 18 15 6
Oleic acid 3 3 3 0 1
AES 1 1 1 5 5
AEO9 8 8 8 8 8
TO8 3 0 0 10 10
Pigment Proper amount of Proper amount of Proper amount of Proper amount of Proper amount of
Essence Proper amount of Proper amount of Proper amount of Proper amount of Proper amount of
Deionized water Balance of Balance of Balance of Balance of Allowance of
Examples 4-6 methods of making laundry beads with germicidal and disinfectant effects were all as follows:
s1, adding PCMX into a mixed solution of polyethylene glycol and other solvents according to the mass fraction, and stirring and dissolving;
s2, sequentially adding a neutralizing agent and dodecyl benzene sulfonic acid, stirring for 10min, and raising the temperature of the solution to 50 ℃ after complete dissolution;
s3, adding an anionic surfactant, stirring for reacting for 20min, then adding a nonionic surfactant, and stirring until the mixture is clear and transparent;
s4, cooling to 45 ℃, adding an auxiliary agent and water, and uniformly stirring to obtain a concentrated solution;
and S5, carrying out film sealing and packaging on the concentrated solution in a film sealing and packaging machine by using polyvinyl alcohol to obtain the washing condensation bead with the sterilization and disinfection effects.
The laundry beads of comparative examples 5-6 differ from examples 4-6 in that: the content of each component in the washing gel bead is changed, and other preparation methods and steps are the same.
Test example 1
Sterilization and disinfection Capacity test
The test method comprises the following steps: the sterilization and disinfection abilities of the laundry beads having sterilization and disinfection effects prepared in examples 1-3 were tested according to QB/T2738 standard method and disinfection specification (2002 edition). The specified test species was selected from staphylococcus aureus, escherichia coli, klebsiella pneumoniae, and candida albicans.
Tests prove that the washing gel bead with the sterilization and disinfection effects has good sterilization and disinfection capacity, the sterilization effect on staphylococcus aureus, escherichia coli, klebsiella pneumoniae and candida albicans is as high as 99.9%, and the disinfection effect is as high as 99.999%.
Test example 2
Test of compressive Capacity
The test method comprises the following steps: the laundry beads prepared in examples 1-3 and comparative examples 1-4 were tested for their compression resistance. A WDS-1 type microcomputer is adopted to control a universal testing machine, a pressure testing mode is entered, fixed-point shutdown is set to be 1000N, a clothes washing coagulated bead sample is heated to be formed upwards, clicking is started, and the machine automatically tests and records a pressure value.
The test results are shown in table 3:
TABLE 3 compression resistance test results
Figure BDA0003725507490000071
Figure BDA0003725507490000081
As can be seen from Table 3, in comparison with comparative example 1 and comparative example 2, the compression resistance value of the product obtained in example 1 is obviously improved by introducing polyethylene glycol 1 and adopting the preferable proportion range; in the comparative example 1, isopropanol is used for replacing glycerol, and the filling degree and the compression resistance value of the appearance of the coagulated beads are not obviously improved. Comparative example 3 is improved in compression resistance value relative to comparative example 2 by increasing the amount of sulfonic acid, but is not much improved in the degree of soft collapse. In comparative example 4, the compression resistance value is significantly improved and the degree of beading and soft collapse is improved as compared with comparative example 3 by increasing the sulfonic acid content to 20%, but the expected effect is not achieved. In the embodiment 2 and the embodiment 3, polyethylene glycol 1 is replaced by polyethylene glycol 2 with different contents (in the preferable proportion range of the technical scheme of the invention), and the dosage of sulfonic acid is increased (in the preferable proportion range of the technical scheme of the invention), so that the compression resistance value of the obtained laundry gel bead is greatly improved and is as high as over 1000N, the appearance of the gel bead is full and stiff, and the improvement effect is obvious.
Test example 3
Stability test
The test method comprises the following steps: stability tests were performed on the laundry beads prepared in examples 4-6 and comparative examples 5-6. The specific investigation indexes of the relevant stability are as follows:
low-temperature stability: the sample was placed in a 0 ℃ freezer for 4 weeks, returned to normal temperature, and observed for appearance.
High-temperature stability: the sample was placed in an oven at 45 ℃ for 4 weeks, returned to normal temperature, and observed for appearance.
High temperature and high humidity stability: the sample was placed in a constant temperature and humidity chamber for 4 weeks (40 ℃/75% humidity), returned to normal temperature, and observed for appearance.
The test results are shown in table 4:
table 4 stability test results
Sample(s) Stability at Low temperature High temperature stability High temperature high humidity stability
Example 4 No delamination and no precipitation No delamination and no precipitation No delamination and no precipitation
Example 5 No delamination and no precipitation No delamination and no precipitation No delamination and no precipitation
Example 6 No delamination and no precipitation No delamination and no precipitation No demixing and no precipitation
Comparative example 5 Demixing and obvious precipitation Demixing and obvious precipitation Demixing and obvious precipitation
Comparative example 6 Severe cloudiness Demixing and obvious precipitation Demixing and obvious precipitation
It can be seen from table 4 that examples 4-6 correspond to good stability of the laundry bead product, but that precipitation stratification occurred during the stability test of comparative examples 5-6. Therefore, the PCMX bactericide is not simply added in the formula of the disinfecting and sterilizing laundry gel bead, and the stability of the laundry gel bead has a large relation with the components and the content thereof in the formula.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it is to be understood that all embodiments may be combined as appropriate by one of ordinary skill in the art to form other embodiments as will be apparent to those of skill in the art from the description herein.

Claims (10)

1. The washing gel bead with the sterilization and disinfection effects is characterized by comprising a content and an outer layer;
wherein the content of the first and second substances,
the content comprises the following components in percentage by mass:
Figure FDA0003725507480000011
water;
the outer layer is a polyvinyl alcohol film.
2. A laundry bead having germicidal and disinfectant effects as claimed in claim 1, wherein said polyethylene glycol has the following general structural formula:
Figure FDA0003725507480000012
wherein n is 2 to 8.
3. A laundry bead with germicidal and disinfectant effects as claimed in claim 1, wherein said contents comprise the following ingredients in mass fraction:
Figure FDA0003725507480000013
Figure FDA0003725507480000021
and (3) water.
4. A laundry bead with germicidal and disinfectant effects as claimed in claim 1, wherein said polyvinyl alcohol film has a thickness of 30-120 μm.
5. A laundry bead with germicidal and disinfectant effects according to claim 1, wherein said other solvent is selected from one or more of glycerol, 1, 2-propanediol, isopropanol, ethanol.
6. A laundry bead having germicidal and disinfectant effects as claimed in claim 1, wherein said anionic surfactant is selected from one or more of sodium fatty alcohol polyoxyethylene sulfate, oleic acid, lauric acid, coconut oil acid.
7. A laundry bead having germicidal and disinfectant effects according to claim 1, wherein said neutralizing agent is selected from one or more of sodium hydroxide, potassium hydroxide, monoethanolamine, diethanolamine, triethanolamine.
8. A laundry bead having germicidal and disinfectant effects according to claim 1, wherein said nonionic surfactant is selected from one or more of fatty alcohol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether, and fatty acid methyl ester ethoxylate.
9. A laundry bead with germicidal and disinfectant effects, as claimed in claim 1, wherein said adjunct is selected from one or more of optical brighteners, enzyme agents, antiredeposition agents, perfumes, pigments.
10. The method for preparing laundry beads with sterilizing and disinfecting effects as claimed in any one of claims 1 to 9, wherein the method for preparing laundry beads with sterilizing and disinfecting effects comprises the following steps:
s1, adding parachlorometaxylenol into a mixed solution of polyethylene glycol and other solvents, and stirring for dissolving;
s2, sequentially adding a neutralizing agent and dodecyl benzene sulfonic acid, stirring and dissolving, and then raising the temperature of the solution;
s3, adding an anionic surfactant, stirring for reaction, then adding a nonionic surfactant, and stirring until the mixture is clear and transparent;
s4, cooling, adding an auxiliary agent and water, and uniformly stirring to obtain a concentrated solution;
and S5, sealing and packaging the concentrated solution by using a polyvinyl alcohol film to obtain the washing gel bead with the sterilization and disinfection effects.
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CN110257182A (en) * 2019-06-21 2019-09-20 广州市百爱神生物科技有限公司 A kind of hyperconcetration fabric washing coagulates pearl and preparation method
CN111733027A (en) * 2020-07-08 2020-10-02 青岛拜士特新材料有限公司 Instant washing antibacterial master batch and preparation method thereof

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CN103451037A (en) * 2013-06-19 2013-12-18 天津科技大学 Sterilization laundry detergent containing epsilon-polylysine
US20160319225A1 (en) * 2015-04-29 2016-11-03 The Procter & Gamble Company Method of treating a fabric
WO2017091674A1 (en) * 2015-11-26 2017-06-01 The Procter & Gamble Company Liquid detergent compositions comprising protease and encapsulated lipase
CN110257182A (en) * 2019-06-21 2019-09-20 广州市百爱神生物科技有限公司 A kind of hyperconcetration fabric washing coagulates pearl and preparation method
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* Cited by examiner, † Cited by third party
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