CN113773916A - Preparation method and application of structured liquid detergent generated in situ - Google Patents
Preparation method and application of structured liquid detergent generated in situ Download PDFInfo
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- CN113773916A CN113773916A CN202011222753.9A CN202011222753A CN113773916A CN 113773916 A CN113773916 A CN 113773916A CN 202011222753 A CN202011222753 A CN 202011222753A CN 113773916 A CN113773916 A CN 113773916A
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
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- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2041—Dihydric alcohols
- C11D3/2044—Dihydric alcohols linear
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
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- C11D3/2003—Alcohols; Phenols
- C11D3/2065—Polyhydric alcohols
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2086—Hydroxy carboxylic acids-salts thereof
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/34—Organic compounds containing sulfur
- C11D3/349—Organic compounds containing sulfur additionally containing nitrogen atoms, e.g. nitro, nitroso, amino, imino, nitrilo, nitrile groups containing compounds or their derivatives or thio urea
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
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- C11D3/382—Vegetable products, e.g. soya meal, wood flour, sawdust
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38618—Protease or amylase in liquid compositions only
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38627—Preparations containing enzymes, e.g. protease or amylase containing lipase
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38645—Preparations containing enzymes, e.g. protease or amylase containing cellulase
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/48—Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/50—Perfumes
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- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
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- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
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- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
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- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/28—Sulfonation products derived from fatty acids or their derivatives, e.g. esters, amides
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- C11D1/29—Sulfates of polyoxyalkylene ethers
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Abstract
The invention relates to a preparation method of a structured liquid detergent, which comprises the following basic steps: dissolving a water-soluble surfactant in a liquid detergent formulation in water and heating; ii, adding structurable substances and uniformly mixing; iii, mechanical shearing and emulsifying; iv, cooling to the crystallization temperature at the speed of 1-3 ℃/min, and keeping the temperature for 0.5-1.5 h; naturally cooling to room temperature; and vi, adding other components and supplementing volatilized water. The method is characterized in that the structured system can be generated in situ by directly relying on the components of the liquid detergent formula, the fiber network structure in the structured system can be completely preserved, the impact and the influence of an external structure system on the detergent formula can be avoided, the method has wide applicability to different detergent formulas, and meanwhile, the manufacturing unit of the external structure system can be omitted, and the equipment investment and the occupied area can be saved.
Description
Technical Field
The invention relates to a preparation method and application of a structured liquid detergent, in particular to a preparation method and application of a structured liquid detergent for in-situ generation of a structured system by relying on a surface active component of the detergent.
Background
Liquid detergents are mainly of two types: unstructured liquid detergents and structured liquid detergents. The aqueous phase of the unstructured liquid wash is isotropic, with the major ingredients being a surfactant of good water solubility, water and other related adjuvants or additives. The structured liquid detergent is a detergent which is added with some insoluble or water-insoluble particle or liquid drop substances on the basis of an unstructured detergent, and the suspended particles are kept in a uniformly dispersed state in the detergent for a long time by adding the structured substances capable of changing the rheological property of a system or by self-assembly of surface active ingredients of the liquid detergent. The particulate or liquid droplet material may be any number of materials which improve the characteristics of the detergent product, such as fluorescent powders, pearlescent agents, bleaching powders, coloured particles and perfume microcapsules. The added functional auxiliary agent particles or liquid drops have the beneficial effects of improving the cleaning capacity of the detergent, visual sense organs and the like.
As mentioned above, the differential nature of unstructured and structured liquid detergents depends critically on whether an external structuring material is added which can alter the rheological properties of the system or whether the functionality of the liquid detergent surfactant self-assembles to create a long lasting stable dispersion of particulate material. Currently, the art is primarily concerned with the preparation of detergent structuring systems by the addition of structurable substances. One structurable substance commonly recognized in the industry is hydrogenated castor oil and there have been many reports of this. For example, patent publication No. CN104685043A discloses an External Structuring System (ESS) comprising a crystalline triglyceride (hydrogenated castor oil), a surfactant and an organic alcohol without amino functional groups, which generates the ESS beforehand by external conditions and then adds to a liquid detergent. Another patent publication CN 109880700 a discloses an external structuring system composition for liquid detergents by adjusting the external conditions to crystallize 12-hydroxy-octadecanoic acid triglyceride (hydrogenated castor oil main component) into fibrous units, which are then mixed with the liquid detergent to form a stable dispersion. Both reports above form structured liquid detergents by pre-forming the external structural system and then adding it to the detergent. However, such methods have the following problems: pre-formed fibrous structuring elements are easily destroyed in industrial applications when pumped in or out through pipe flow, resulting in a decrease in the efficiency of suspension stabilization or an increase in costs due to the need to use larger amounts of external structuring systems; the preparation of external structural systems often requires the use of high concentrations of surfactants and some organic solvents, which tend to impact the formulation system of the detergent itself and cause changes in the properties of the final product; additional preparation equipment is required, increasing equipment cost and floor space.
It is therefore an object of the present invention to provide a process for the preparation of liquid detergents with in situ generation of a structuring system, i.e. a structuring system with in situ generation of a system with variable rheology properties directly by means of detergent manufacturing equipment and its own formulation ingredients without the need for additional manufacturing equipment units; the problems presented above are well solved.
Disclosure of Invention
The present invention relates to a process for the preparation of a structured liquid detergent with in situ generation of a structuring system, said process comprising the steps of:
dissolving a water-soluble surfactant in water according to a liquid detergent formula, stirring and mixing uniformly, and heating to the melting point of a structurable substance or a temperature above the melting point, preferably deionized water;
ii, adding the structurable substance into the mixture in i and stirring until the structurable substance is dissolved or uniformly mixed;
emulsifying the structurable substance by high-strength mechanical stirring to form uniform emulsion;
iv, cooling the emulsion in the iii to the crystallization temperature of the structurable substance at a controlled cooling rate of 1-3 ℃/min under slow stirring, and keeping the temperature for 0.5-1.5 h;
standing or stirring at a slow speed, and naturally cooling to 15-35 ℃;
adding insoluble or insoluble granular substances and other optional added components in the liquid detergent formula, supplementing the balance and volatile water, and uniformly mixing;
the method is characterized in that: the structuring system is generated in situ directly from and interacting with the liquid detergent formulation components themselves.
The liquid detergent is a liquid composition consisting of a surfactant, water and other auxiliaries or additives. Wherein the surfactant comprises 0% to 95%, preferably 10% to 75%, most preferably 15% to 45% by weight of the liquid detergent.
The surfactant is one or more of anionic surfactant, nonionic surfactant, cationic surfactant and amphoteric surfactant.
The anionic surfactant is one or a mixture of more of Linear Alkylbenzene Sulfonate (LAS), sodium branched alkylbenzene sulfonate (ABS), fatty alcohol polyoxyethylene ether sulfate (AES), alpha-sulfo fatty acid ester salt (MES), sulfonate of fatty acid methyl ester ethoxylate (FMES), fatty Alcohol Ether Carboxylate (AEC), alpha-olefin sulfonate (AOS), dodecyl sulfonate (SDS), Secondary Alkyl Sulfonate (SAS), lauryl ether sulfonate, lignosulfonate and natural plant extract.
The nonionic surfactant is one or a mixture of more of fatty alcohol-polyoxyethylene ether (AEO), alkyl glycoside (APG), Fatty Acid Alkanolamide (FAA), nonylphenol polyoxyethylene ether (TX-n), alkylamine oxide, cocoamidol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyalcohol polymer, polyethylene glycol terephthalate and natural plant extract.
The cationic surfactant is one or more of sLalammonium chloride, benzalkonium chloride, quaternary ammonium compounds, amine compounds and vinyl oxide sulfate.
The amphoteric surfactant is one or more of amino acid type, betaine type and imidazoline type.
The structurable substance is a crystallizable glyceride, preferably a crystalline hydroxystearic acid triglyceride, most preferably hydrogenated castor oil; the weight percentage of the detergent is 0.1-1%, preferably 0.2-0.5%.
The insoluble or water insoluble particulate matter includes, but is not limited to, one or more mixtures of colored particulates, pigments, bleaching powders, phosphors, microcapsules, pearlescent agents, and suds suppressors.
Other optional additional ingredients in the liquid detergent formulation include, but are not limited to, one or more mixtures of builders, pH adjusting agents, chelating agents, soil suspending agents, fabric care agents, solubilizers, enzymes, enzyme stabilizers, preservatives, suds suppressors, colorants, dye transfer inhibitors.
The structuring system refers to the overall structural distribution of the liquid detergent with a microscopic network structure inside, which can influence and change the viscosity and yield stress of the detergent, and further change the overall suspending capacity.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the liquid detergent for in-situ generation of the structured system does not need to use an external structure system manufacturing unit, can rely on the components of the detergent formula to generate the structured system in situ, has wide applicability of different detergent formulas, and can save equipment investment and floor area;
the preparation method of the liquid detergent for in-situ generation of the structured system saves the operation processes of storage, pumping, addition and the like in industrial application, and can completely preserve the fiber network structure in the structured system;
the liquid detergent preparation method for in situ generation of the structuring system according to the present invention generates the structuring system by relying on the components of the detergent formulation itself, thus avoiding the introduction of a large amount of other ingredients and avoiding the impact and influence of external structuring systems on the detergent formulation itself.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to the following examples.
Configuration of structured liquid detergent:
according to the formula table of examples 1-4 in the table 1-4, a water-soluble surfactant in a liquid detergent is firstly added into deionized water and stirred until the water-soluble surfactant is completely dissolved, stirred and mixed uniformly, and heated to 95 ℃;
ii, adding hydrogenated castor oil powder into the mixture in the step i, and stirring until the hydrogenated castor oil powder is dissolved or uniformly mixed;
iii, carrying out high-strength mechanical shearing stirring on the mixed solution formed in the ii for 5min to form uniform emulsion;
iv, cooling the emulsion in the iii to 70 ℃ at a cooling rate of 1 ℃/min under slow stirring, and keeping the temperature of the emulsion in the examples 1-4 for 0.75h, 1h, 1.25h and 1.5h respectively;
standing and naturally cooling to 25 ℃;
vi, adding other components in the formula tables of the examples 1 to 4 in the tables 1 to 4, supplementing the balance and the volatilized water, and uniformly mixing;
collecting to obtain the structured liquid detergent prepared by the method.
Configuration of unstructured liquid detergent:
according to the formula table of comparative examples 1-4 in tables 1-4, water-soluble components in the liquid detergent are firstly added into deionized water and stirred until the water-soluble components are completely dissolved, then the required surfactant is added, and the mixture is stirred and mixed uniformly; adding the other components in the table, and stirring and mixing uniformly; collecting to obtain the unstructured liquid detergent.
And (3) testing yield stress: testing with Brookfield RST rheometer at 25 deg.C with shear rate scanning range of 0-200S-1Stability index R, fitting by the Herschel-Bulkley model2It should be greater than 0.999.
And (3) suspension stability test: the liquid detergents corresponding to examples 1 to 4 and comparative examples 1 to 4, which were in equal amounts, were respectively subjected to a high temperature stability test, a low temperature stability test, a normal temperature stability test and a freeze-thaw cycle stability test.
High-temperature stability: and placing the test sample in an environment of 40 +/-1 ℃, after placing for 1 month at constant temperature, recovering to the room temperature of 25 +/-5 ℃, and observing appearance change conditions, wherein if no layering, precipitation or agglomeration phenomenon exists, the high-temperature stability is qualified.
Low-temperature stability: and placing the test sample in an environment of 0 +/-2 ℃, standing at constant temperature for 1 month, taking out, and immediately observing the appearance change condition, wherein if no layering, precipitation or agglomeration phenomenon exists, the low-temperature stability is qualified.
And (3) normal temperature stability: and (3) placing the test sample in a room temperature environment (20-30 ℃), standing at a constant temperature for 1 month, and immediately observing the appearance change condition, wherein if no layering, precipitation or agglomeration phenomenon exists, the normal temperature stability is qualified.
Freeze-thaw cycle stability: placing a test sample in an environment of-15 to-20 ℃, standing at a constant temperature for 24 hours, taking out, placing in an environment of 25 +/-5 ℃ at room temperature for 24 hours, circulating for one time, continuously circulating for five times, observing the state of the composition each time, and if no layering, precipitation or agglomeration phenomenon exists after five times of circulation, the freeze-thaw cycle stability is qualified.
TABLE 1
TABLE 2
TABLE 3
TABLE 4
As can be seen from the results in tables 1-4, the structured liquid detergents prepared by the method of the present invention have no delamination, precipitation or agglomeration after the high temperature stability, low temperature stability, normal temperature stability and freeze-thaw cycle stability tests, yield stress values are maintained at a high level, and the structured liquid detergents have wide applicability to different detergent formulations, while the unstructured liquid detergents not prepared by the method of the present invention in the comparative examples show respectively the phenomena of unstable suspension and no yield stress measurement, and thus the liquid detergents in which the structured systems are generated in situ depending on the components of the detergent formulation of the present invention can have strong suspension ability, and have very wide practical application values.
The embodiments described above are merely specific embodiments of the present invention, and various changes and modifications may be made to the present invention without departing from the spirit and scope of the present invention, which fall within the scope of the claimed invention.
Claims (13)
1. A method for preparing a structured liquid detergent for in situ generation of a structured system comprises the following specific steps:
dissolving a water-soluble surfactant in water according to a liquid detergent formula, stirring and mixing uniformly, and heating to the melting point of a structurable substance or a temperature above the melting point, preferably deionized water;
ii, adding the structurable substance into the mixture in i and stirring until the structurable substance is dissolved or uniformly mixed;
emulsifying the structurable substance by high-strength mechanical stirring to form uniform emulsion;
iv, cooling the emulsion in the iii to the crystallization temperature of the structurable substance at a controlled cooling rate of 1-3 ℃/min under slow stirring, and keeping the temperature for 0.5-1.5 h;
standing or stirring at a slow speed, and naturally cooling to 15-35 ℃;
adding insoluble or insoluble granular substances and other optional added components in the liquid detergent formula, supplementing the balance and volatile water, and uniformly mixing;
the process of manufacture is characterised in that the structuring system is generated in situ directly from and interacting with the liquid detergent formulation components themselves.
2. The liquid detergent according to claim 1, wherein the liquid detergent is a liquid composition consisting of a surfactant, water and other auxiliaries or additives.
3. A liquid detergent according to claim 2 characterised in that the surfactant comprises from 0% to 95%, preferably from 10% to 75%, most preferably from 15% to 45% by weight of the liquid detergent.
4. A liquid detergent according to claim 3 wherein the surfactant is a mixture of one or more of anionic, nonionic, cationic and amphoteric surfactants.
5. The surfactant according to claim 4, wherein the anionic surfactant is one or more of Linear Alkylbenzene Sulfonate (LAS), sodium branched alkylbenzene sulfonate (ABS), fatty alcohol polyoxyethylene ether sulfate (AES), alpha-sulfo fatty acid ester salt (MES), sulfonate of fatty acid methyl ester ethoxylate (FMES), fatty Alcohol Ether Carboxylate (AEC), alpha-alkenyl sulfonate (AOS), dodecyl sulfonate (SDS), Secondary Alkyl Sulfonate (SAS), lauryl ether sulfonate, lignosulfonate and natural plant extracts.
6. The surfactant of claim 4, wherein said nonionic surfactant is one or more selected from the group consisting of fatty alcohol polyoxyethylene ether (AEO), alkyl glycoside (APG), Fatty Acid Alkanolamide (FAA), nonylphenol polyoxyethylene ether (TX-n), alkylamine oxide, cocoamidol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyol polymer, polyethylene terephthalate, and natural plant extracts.
7. The surfactant of claim 4, wherein the cationic surfactant is one or more of the group consisting of seleonium chloride, benzalkonium chloride, quaternary ammonium compounds, amine compounds, and vinyl oxide sulfates.
8. The surfactant according to claim 4, wherein the amphoteric surfactant is a mixture of one or more of amino acid type, betaine type and imidazoline type.
9. A method according to claim 1, characterised in that the structurable substance is a crystallizable glyceride, preferably a crystalline hydroxystearic acid-containing triglyceride, most preferably hydrogenated castor oil.
10. Structurable substance according to claim 9, characterized in that it represents 0.1% to 1%, preferably 0.2% to 0.5% by weight of the liquid detergent.
11. The method of claim 1, wherein the insoluble or water-insoluble particulate material comprises one or more of a mixture of, but not limited to, colored particles, pigments, bleaching powders, fluorescent powders, microcapsules, pearlescers, and suds suppressors.
12. The process of claim 1, wherein the other optional adjunct ingredients in the liquid detergent formulation include, but are not limited to, one or more mixtures of builders, pH adjusting agents, chelating agents, soil suspending agents, fabric care agents, solubilizing agents, enzymes, enzyme stabilizers, preservatives, suds suppressors, colorants, dye transfer inhibitors.
13. The method of claim 1, wherein the structuring system is a microstructure within the liquid detergent that alters the viscosity and yield stress of the liquid detergent and thus the overall suspension capacity.
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CN115612568A (en) * | 2022-09-30 | 2023-01-17 | 广州蓝月亮实业有限公司 | Stable structured detergent composition |
CN115926902A (en) * | 2022-12-30 | 2023-04-07 | 中山榄菊日化实业有限公司 | Suspending agent for stabilizing microcapsule essence in laundry detergent and prepared laundry detergent |
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