CN115926896B - High viscosity water-soluble unit dose detergent compositions and methods of making same - Google Patents
High viscosity water-soluble unit dose detergent compositions and methods of making same Download PDFInfo
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- CN115926896B CN115926896B CN202211361275.9A CN202211361275A CN115926896B CN 115926896 B CN115926896 B CN 115926896B CN 202211361275 A CN202211361275 A CN 202211361275A CN 115926896 B CN115926896 B CN 115926896B
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- 239000003599 detergent Substances 0.000 title claims abstract description 35
- 239000000203 mixture Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title abstract description 5
- 229920000642 polymer Polymers 0.000 claims abstract description 35
- 239000002562 thickening agent Substances 0.000 claims abstract description 30
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 29
- 239000002904 solvent Substances 0.000 claims abstract description 28
- 239000003223 protective agent Substances 0.000 claims abstract description 24
- 239000004094 surface-active agent Substances 0.000 claims abstract description 18
- 125000005396 acrylic acid ester group Chemical group 0.000 claims abstract description 6
- 239000000839 emulsion Substances 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- -1 acrylic acid/ester compound Chemical class 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- 239000000178 monomer Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000003945 anionic surfactant Substances 0.000 claims description 6
- 239000002736 nonionic surfactant Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 5
- 235000011054 acetic acid Nutrition 0.000 claims description 5
- 239000002280 amphoteric surfactant Substances 0.000 claims description 5
- 239000011324 bead Substances 0.000 claims description 5
- 235000015165 citric acid Nutrition 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- 239000004310 lactic acid Substances 0.000 claims description 5
- 235000014655 lactic acid Nutrition 0.000 claims description 5
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 239000011975 tartaric acid Substances 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 239000003094 microcapsule Substances 0.000 claims description 4
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 claims description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 3
- 230000002209 hydrophobic effect Effects 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 239000008188 pellet Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000002156 mixing Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 2
- 239000003607 modifier Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 15
- 239000007788 liquid Substances 0.000 description 10
- 238000007789 sealing Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000005491 wire drawing Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000002191 fatty alcohols Chemical class 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000002888 zwitterionic surfactant Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- RFIMISVNSAUMBU-UHFFFAOYSA-N 2-(hydroxymethyl)-2-(prop-2-enoxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC=C RFIMISVNSAUMBU-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- JNGWKQJZIUZUPR-UHFFFAOYSA-N [3-(dodecanoylamino)propyl](hydroxy)dimethylammonium Chemical compound CCCCCCCCCCCC(=O)NCCC[N+](C)(C)[O-] JNGWKQJZIUZUPR-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229940086737 allyl sucrose Drugs 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- MRUAUOIMASANKQ-UHFFFAOYSA-N cocamidopropyl betaine Chemical compound CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC([O-])=O MRUAUOIMASANKQ-UHFFFAOYSA-N 0.000 description 1
- 229940073507 cocamidopropyl betaine Drugs 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 229940047642 disodium cocoamphodiacetate Drugs 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000006081 fluorescent whitening agent Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 1
- 229940026210 lauramidopropylamine oxide Drugs 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Landscapes
- Detergent Compositions (AREA)
Abstract
The present invention discloses a high viscosity water-soluble unit dose detergent composition. Having a sachet made of a water-soluble film, the sachet having at least one closed chamber enclosing contents therein; the content is formed by blending an A phase component and a B phase component; wherein the phase a component comprises at least a solvent and an alkaline modifier, based on the total mass of the encapsulated contents; the phase B component at least comprises a solvent, a polymer thickener and a carboxyl protecting agent; the polymer type thickener is emulsion or powdery acrylic acid/ester polymer; surfactants are also included, added in the a-phase component, or in the B-phase component, or in the a-phase and B-phase components, respectively. Its preparing process is also disclosed. The invention can effectively solve the technical problem that the water-soluble unit dose detergent is difficult to inject high-viscosity content in the production process.
Description
Technical Field
The invention belongs to the technical field of daily detergents, and particularly relates to a high-viscosity water-soluble unit-dose detergent composition and a preparation method thereof.
Background
The washing product with water-soluble unit dosage such as laundry gel beads is a novel detergent which wraps the content by utilizing a water-soluble polymer film, and has a certain share in the detergent market at home and abroad because of the advantages of convenient use, attractive appearance, diversified functions and the like. According to different application scenes and washing objects, the wrapped content of the detergent is liquid, powder, particles or even detergent blocks. The contents rarely have a high viscosity state due to the limitations of production equipment and processes. While a high viscosity matrix can give the consumer a more concentrated look and feel; some water-soluble unit dose detergent products will incorporate water-insoluble functional materials (such as microcapsules, pearly-lustre powder, pearly-lustre pulp, petals etc.), while higher system viscosity can reduce the sedimentation rate of the object, which is beneficial to maintain the stability of the system.
The general production process of water-soluble unit dose detergents is: firstly, the water-soluble film is deformed by vacuum and is adsorbed on the inner side of a groove of a die, then, the detergent is injected into the groove through a liquid injection nozzle, and then, the film is directly sealed or the contents of other cavities are continuously injected according to the design of single cavity or multiple cavities. Currently, for single-or multi-chamber unit dose detergent products, the same chamber contents are injected in a substantially all-disposable manner. During the filling, if the detergent is a liquid having a relatively high viscosity, a "stringing" phenomenon may occur above the filling nozzle and the groove. The "stringing" phenomenon may lead to two negative effects: on the one hand, the retention time of the liquid injection nozzle can be adjusted and lengthened due to the fact that the wire drawing is required to wait for breakage, so that the liquid injection efficiency is reduced; on the other hand, during nozzle residence, part of the "stringing" does not break and accidentally splash the liquid contents onto the film seal location, affecting the seal effect and even causing leakage of unit dose product. Therefore, how to prepare a unit dose detergent that produces a content having a high viscosity is a technical problem that needs to be solved in the art.
Disclosure of Invention
It is a first object of the present invention to provide a high viscosity water soluble unit dose detergent composition which effectively addresses the deficiencies of the prior art.
It is a second object of the present invention to provide a process for preparing the high viscosity water soluble unit dose detergent composition.
In order to achieve the first object, the invention adopts the following technical scheme:
A high viscosity water soluble unit dose detergent composition having a sachet made of a water soluble film, said sachet having at least one closed chamber enclosing the contents therein; the content is formed by blending an A phase component and a B phase component; wherein, based on the total mass of the encapsulated content, the A phase component at least comprises 10-50% of solvent and 0.1-5% of alkaline regulator by mass percent; the phase B component at least comprises 10-60% of solvent, 1-25% of polymer thickener and 0-4% of carboxyl protective agent by mass percent; the polymer type thickener is emulsion or powdery acrylic acid/ester polymer; the total mass percentage of the solvent is 20-71%; the composite material also comprises 21-60% of surfactant by mass, wherein the surfactant is added into the A phase component, the B phase component or the A phase component and the B phase component respectively.
Preferably, the polymer thickener is polymerized by using an acrylic acid/ester compound as a monomer and other monomers having a hydrophobic compound and/or monomers having an amphiphilic compound. More preferably, the molecular chain of the polymer thickener has an ionizable hydrophilic group, which includes a carboxyl group.
Preferably, the viscosity of the content is not less than 1000 mPa.S and the pH is 6.5-8.5.
Further, the multifunctional food also comprises a water-insoluble functional substance, wherein the water-insoluble functional substance is one of microcapsules, oil drop essence, petal gel, pearl powder, pearl slurry, micropill and soft bead, or the combination of at least two of the two; the water-insoluble functional substance is added to the A-phase component, or to the B-phase component, or to the A-phase component and the B-phase component, respectively.
Preferably, the alkaline regulator is one of sodium hydroxide, potassium hydroxide, monoethanolamine and triethanolamine, or a combination of at least two of them; the dosage of the carboxyl protecting agent is not zero, and the carboxyl protecting agent is one of citric acid, oxalic acid, tartaric acid, lactic acid, formic acid, acetic acid and sulfamic acid, or the combination of at least two of the citric acid, oxalic acid, tartaric acid, lactic acid, formic acid, acetic acid and sulfamic acid; the solvent is one of water, ethanol, ethylene glycol, propylene glycol, glycerol, diethylene glycol, dipropylene glycol, polyethylene glycol, polypropylene glycol, dipropylene glycol butyl ether and sorbitol, or a combination of at least two of the two; the surfactant is one of anionic surfactant, nonionic surfactant and amphoteric surfactant, or the combination of at least two of them.
Preferably, the phase A component comprises 20 to 59.9 mass percent of surfactant, 10 to 50 mass percent of solvent, 0.1 to 5 mass percent of alkaline regulator and 0.1 to 1.5 mass percent of water-insoluble functional substance; the phase B component comprises 0.1-20% of surfactant, 10-60% of solvent, 1-25% of polymer thickener and 0-4% of carboxyl protecting agent by mass percent.
In order to achieve the second purpose, the invention adopts the following technical scheme:
a process for preparing a high viscosity water soluble unit dose detergent composition as described above, comprising the steps of:
1) Respectively preparing an A phase component and a B phase component;
2) Injecting the phase A component and the phase B component into a mold cavity for preparing a single bag sequentially or simultaneously;
3) After the finished product of the product is prepared, the finished product of the product is vibrated for 10 to 50 seconds at the frequency of 50 to 300 times per minute with the amplitude of 5 to 20mm, so that the A phase component and the B phase component are completely mixed; or naturally storing to completely mix the A phase component and the B phase component.
Preferably, the preparation steps of the phase B component are as follows:
11 Adding a carboxyl protecting agent into a solvent, and adjusting the pH value to be not more than 6.0;
12 Pre-dissolving and dispersing the polymer thickener by the solvent obtained in the step 11), and uniformly stirring;
13 Then adding the rest components to obtain a B phase component;
The pH of the polymeric thickener is not greater than 6.5.
Preferably, the pH of the A phase component is 7.5-10.5, and the pH of the B phase component is 3.0-6.0; the weight ratio of the phase A component to the phase B component is 2:8-8:2; the viscosity of the A-phase component is not more than 800 mPa.S; the viscosity of the B phase component is not more than 800 mPa.S.
By adopting the technical scheme, the technical problem that the water-soluble unit dose detergent is difficult to inject high-viscosity content in the production process can be effectively solved; the high viscosity of the content can also help the suspension of the water-insoluble functional substances, so that the product is endowed with more novel and fashionable visual impression.
Detailed Description
The invention is further described below with reference to examples.
In the following examples, the viscosities are the absolute viscosity of the newtonian fluid and the apparent viscosity of the non-newtonian fluid, as measured by a rotational viscometer at 25 ℃. The viscometer speed was fixed at 12 rpm, taking into account the apparent viscosity of the non-newtonian fluid as a function of shear force. To determine the viscosity state of the encapsulated unit dose detergent product contents, it is necessary to manually shear the encapsulated and fully reacted unit dose detergent product through the sealing membrane and pour the contents out, the contents accumulating at least 100mL.
The invention divides the content in the detergent bag of unit dose into a phase A component and a phase B component with low viscosity and respectively prepares the components, and then the components are injected into a mould simultaneously or in two times; after the membrane is encapsulated, the two-phase components react in the cavity to form a content with high viscosity, so that the problem that the high-viscosity filler is difficult to produce is solved, and the suspension stability of the water-insoluble functional substance is improved.
The preparation method of the high-viscosity water-soluble unit dose detergent composition comprises the following steps:
1) The low viscosity A phase component and B phase component are formulated separately. Wherein the phase A comprises the following components in percentage by mass: 20 to 60 percent of surfactant, 10 to 55 percent of solvent, 0.1 to 5 percent of alkaline regulator and 0.1 to 5 percent of water insoluble functional substance. The phase B contains 0.1-20% of surfactant, 10-60% of solvent, 0-4% of carboxyl protecting agent and 1-25% of polymer thickener.
2) Injecting the phase A component and the phase B component into a mold cavity for preparing a single bag sequentially or simultaneously;
3) After the encapsulation film is prepared into a finished product, oscillating equipment such as a shaking table, a mixer, a vibrating screen and the like is used for carrying out oscillating treatment on the finished product for 10-50 seconds at the amplitude of 5-20 mm and the frequency division rate of 50-300 times; or naturally stored to obtain a high viscosity content.
The viscosity of the above A-phase component and B-phase component should be not more than 800 mPas, more preferably not more than 600 mPas. The viscosity of the finished product content of the product should be not less than 1000 mPa.S, and the viscosity is more preferably in the range of 5000-30000 mPa.S.
The polymer thickener is emulsion or powder acrylic acid/ester polymer, and is polymerized by taking acrylic acid/ester compound as monomer (one of them) and other hydrophobic compound monomer and/or amphipathic compound monomer. Other monomers than the acrylic compounds include: allyl ether compound, allyl sucrose, allyl pentaerythritol, alkyl methacrylic acid, alkanol acrylic ester, styrene and N, N' -methylene bisacrylamide. Further, the polymeric thickener may be selected from the group consisting of road blondAqua SF-1 Polymer、/>ETD 2020 Polymer、/>L-10 Polymer、/>L-20 Polymer, and Gramineae Volarest TM FL. In addition, the acrylic acid/ester polymer preferably has an ionizable hydrophilic group such as a carboxyl group in the molecular chain, and the raw material pH is 6.5 or less.
The preferable preparation steps of the phase B component are as follows: 11 Adding a carboxyl protecting agent to the solvent, and confirming that the pH is adjusted to 6.0 or less; 12 Pre-dissolving and dispersing the polymer thickener by using the solvent obtained in the step 11), and uniformly stirring; 13 Adding the rest components to obtain a phase B component.
The pH value of the A phase component is preferably controlled to be 7.5-10.5, the pH value of the B phase component is controlled to be 3.0-6.0, the weight ratio of the two phases is 2:8-8:2, and the weight ratio is more preferably 4:6-6:4.
After the A phase component and the B phase component are fully mixed, the pH of the finished product of the product is preferably between 6.5 and 8.5.
The water insoluble functional substance in the phase A component is at least one of microcapsule, oil drop essence, petal gel, pearl powder, pearl slurry, micropill and soft bead.
The alkaline regulator is at least one of sodium hydroxide, potassium hydroxide, monoethanolamine and triethanolamine.
Since the carboxyl groups in the acrylic acid/ester polymer are neutralized to give high viscosity and affect normal production, it is preferable to add a proper amount of a carboxyl protecting agent to the preparation of the B phase component to ensure that the carboxyl groups do not react with other compounds in the B phase component before mixing with the A phase component. The carboxyl protecting agent is one or more of citric acid, oxalic acid, tartaric acid, lactic acid, formic acid, acetic acid and sulfamic acid.
The solvent in the phase A component and the phase B component comprises water, ethanol, ethylene glycol, propylene glycol, glycerol, diethylene glycol, dipropylene glycol, polyethylene glycol, polypropylene glycol, dipropylene glycol butyl ether, sorbitol and mixtures thereof.
The surfactant in the above-mentioned a-phase component and B-phase component contains at least one of an anionic surfactant, a nonionic surfactant and an amphoteric surfactant. Wherein the anionic surfactant is one or more of C8-C18 alkylbenzene sulfonate, fatty alcohol polyoxyethylene sulfate, fatty alcohol polyoxyethylene ether carboxylate, alpha-olefin sulfonate, fatty acid salt and fatty acid methyl ester sulfonate. The nonionic surfactant is one or more of fatty alcohol polyoxyalkyl ether, C8-C16 alkyl glycoside, fatty acid methyl ester ethoxylate and grease ethoxylate. The zwitterionic surfactant may be selected from one or more of betaine type, imidazoline type and amine oxide type zwitterionic surfactants. Further, the zwitterionic surfactant is selected from one or more of cocamidopropyl betaine, lauramidopropyl amine oxide, and disodium cocoamphodiacetate.
In addition, one or more of enzyme preparation, chelating agent, fluorescent whitening agent, essence, pigment and antiseptic can be added into the product content.
It should be noted that, the bag of the present invention may also adopt a laundry bead structure with a communicating cavity as disclosed in chinese patent 202120635173.6, i.e. the closed cavity of the present invention is composed of two subchambers and a communicating cavity for communicating the two subchambers. In the preparation process, the A phase component and the B phase component can be injected into one subchamber simultaneously and respectively, and the blending is realized through the communicating cavities.
Examples 1 to 4
Examples 1 to 4 employ thickeners ofAqua SF-1. The proportions of the components of the products of the four examples and the three comparative examples and the relevant performance parameters are shown in Table 1.
The specific preparation methods of the four examples and the three comparative examples are as follows:
1. Preparing a phase A component: adding a solvent and an alkaline regulator into a reaction kettle, and uniformly stirring; then adding anionic surfactant, stirring uniformly, then adding nonionic surfactant and amphoteric surfactant, regulating pH to meet regulation, adding water-insoluble functional material and preservative, and finally measuring final pH and viscosity.
Preparing a phase B component: and regulating the pH of the propylene glycol serving as a solvent to be less than 6.0 by utilizing a carboxyl protective agent, then adding a polymer thickener, dispersing and dissolving the polymer thickener, uniformly stirring the mixture, then adding other components, and finally measuring the final pH and viscosity.
The preparation method of the phase B component of the comparative example 3 is as follows: firstly, uniformly mixing the solvent propylene glycol and the polymer thickener, then adding other components except the carboxyl protecting agent, uniformly stirring, and finally adding the carboxyl protecting agent.
2. Filling and sealing the film on the machine: the water-soluble film is deformed by vacuum and adsorbed on the inner side of a groove of the die, then the A phase component and the B phase component are sequentially injected into the same die cavity of the die through a nozzle, and the single finished product is cut after film sealing. Placing the finished products on a shaking table, and vibrating for 10-50 seconds at the amplitude of 5-20mm and the frequency division rate of 50-300 times.
TABLE 1
It can be seen from table 1 that the difference between example 1 and comparative example 1 is whether or not a polymeric thickener is added to the B phase component. From the petal state of the two, the phase B component of comparative example 1 does not have the effect of stabilizing petals because the polymer type thickening agent is not added, and the product is settled after being placed for one day at room temperature. Whereas example 1 had a higher viscosity and was able to maintain a good appearance over a long period of time.
Comparative example 2 is a sample in which the A phase component was not alkaline-adjusted, and comparative example 3 is a sample in which the B phase component was not added with the carboxyl protecting agent first. From the encapsulation state of comparative example 2, it is known that, for a product with a pH not adjusted to a reasonable range, even if the a-phase component and the B-phase component are sequentially injected into the unit dose cavity according to the preparation method, the formulation can cause phenomena of liquid leakage, wire drawing and the like in the production process, thereby affecting normal production. In comparative example 3, although the pH of the phase B component was also adjusted to 6.0 or less in the latter stage, the carboxyl group thereof was reacted with other compounds to form a phase B having a high viscosity because the carboxyl group protecting agent was not added first, and then the polymer type thickener was directly agglomerated even though the carboxyl group protecting agent was added. Thus, the composition of the present invention requires a strictly defined production process, otherwise even the same combination, pH, would lead to failure of production.
Examples 2, 3 and 4 are different weight ratios of the a phase component to the B phase component of the unit dose composition. From the results, the weight ratio between the A and B phases of the composition is not limited, but the reaction ratio is designed to be within the range after the A, B phases are added in proportion, so that the unit dose detergent product can be normally encapsulated and has the petal stabilizing effect.
Furthermore, in example 4, the total surfactant content was only 21%, indicating that the invention can be implemented in either conventional or concentrated unit dose detergents.
Examples 5 to 6
Examples 5 to 6 employ thickeners which are pulverulentETD 2020 Polymer. The proportions of the product components of the two examples and the three comparative examples and the relevant performance parameters are shown in Table 2.
The specific preparation methods of the two examples and the three comparative examples are as follows:
1. Preparing a phase A component: adding a solvent and an alkaline regulator into a reaction kettle, and uniformly stirring; then adding anionic surfactant, stirring uniformly, then adding nonionic surfactant and amphoteric surfactant, regulating pH to meet regulation, adding water-insoluble functional material and preservative, and finally measuring final pH and viscosity.
Preparing a phase B component: adjusting the pH of the pure water to below 6.0 by using a carboxyl protective agent; then spreading the powdery polymer thickener in the liquid, standing and wetting, and uniformly stirring. Finally, the remaining components are added and the final pH and viscosity are determined.
2. Filling and sealing the film on the machine: the water-soluble film is deformed by vacuum and adsorbed on the inner side of a groove of the die, then the A phase component and the B phase component are sequentially injected into the same die cavity of the die through a nozzle, and the single finished product is cut after film sealing. Placing the finished products on a shaking table, and vibrating for 10-50 seconds at the amplitude of 5-20mm and the frequency division rate of 50-300 times.
TABLE 2
From the state of the water-insoluble functional substances of example 5 and comparative example 4, by the method for preparing a high-viscosity water-soluble unit dose detergent described in the present invention,ETD 2020 Polymer can also be used in unit dose products and function to thicken and suspend particles.
From the analyses of example 6 and comparative example 5, in comparative example 5, both the phase A and phase B of the composition were controlled to be within the range of pH, but since neutralization of the two phases was not properly adjusted after the addition in proportion, the encapsulation was affected and the preparation was not normally performed, the limitation of pH and the ratio of the two phases was required in the present invention, and the effect of the present invention was not achieved by simply adjusting the pH. Comparative example 6 was prepared by mixing phase a and phase B to form the same phase, and then packaging the same phase. However, because the viscosity of the mixed two phases is too high, the phenomenon of 'wiredrawing' is generated when the liquid injection nozzle injects liquid, and the encapsulation is problematic, the invention can effectively avoid the phenomenon of 'wiredrawing' in production and obtain a high-viscosity unit dose washing product.
Examples 7 to 9
In example 7, since only the solvent, the thickener and a smaller amount of the surfactant were contained in the B-phase component, the present invention could be realized even without adding the carboxyl protecting agent,ETD 2020 Polymer can also be used in unit dose products and function to thicken and suspend particles. In examples 8 and 9, since 8% of C8-C14 alkyl glycoside is added, the raw material is more basic, and therefore more acidic protecting agent must be added to ensure that the viscosity is kept low before A, B phases are mixed. In example 9, the present invention was also achieved when the surfactant content in the phase A was 40% or more and the viscosity was reduced to 800 mPas or less by adjusting the ratio of the surfactant in the formulation.
Claims (6)
1. A high viscosity water soluble unit dose detergent composition having a sachet made of a water soluble film, said sachet having at least one closed chamber enclosing a content wherein said content is blended from a phase a and a phase B component; wherein, based on the total mass of the encapsulated contents,
The phase A component at least comprises 10-50% of solvent and 0.1-5% of alkaline regulator in percentage by mass;
the phase B component at least comprises 10-60% of solvent, 1-25% of polymer thickener and 0-4% of carboxyl protective agent by mass percent; the polymer type thickener is emulsion or powdery acrylic acid/ester polymer;
The total mass percentage of the solvent is 20-71%;
The composite material also comprises 21-60% of surfactant by mass, wherein the surfactant is added into the A phase component, or into the B phase component, or into the A phase component and the B phase component respectively;
The viscosity of the content is not less than 1000 mPa.S, and the pH is 6.5-8.5;
The preparation method of the high-viscosity water-soluble unit dose detergent composition comprises the following steps:
1) Respectively preparing an A phase component and a B phase component;
2) Injecting the phase A component and the phase B component into a mold cavity for preparing a single bag sequentially or simultaneously;
3) After the finished product of the product is prepared, the finished product of the product is vibrated for 10 to 50 seconds at the frequency of 50 to 300 times per minute with the amplitude of 5 to 20mm, so that the A phase component and the B phase component are completely mixed; or naturally storing to completely mix the A phase component and the B phase component;
the preparation steps of the phase B component are as follows:
11 Adding a carboxyl protecting agent into a solvent, and adjusting the pH value to be not more than 6.0;
12 Pre-dissolving and dispersing the polymer thickener by the solvent obtained in the step 11), and uniformly stirring;
13 Then adding the rest components to obtain a B phase component;
the pH of the polymeric thickener is no greater than 6.5;
The pH of the A phase component is 7.5-10.5, and the pH of the B phase component is 3.0-6.0; the weight ratio of the phase A component to the phase B component is 2:8-8:2;
the viscosity of the A-phase component is not more than 800 mPa.S; the viscosity of the B phase component is not more than 800 mPa.S.
2. The high viscosity water-soluble unit dose detergent composition according to claim 1, wherein the polymer type thickener is polymerized with other monomers having a hydrophobic compound and/or monomers having an amphiphilic compound by using an acrylic acid/ester compound as a monomer.
3. The high viscosity water-soluble unit dose detergent composition according to claim 2, wherein said polymeric thickener has an ionizable hydrophilic group on a molecular chain, said hydrophilic group comprising a carboxyl group.
4. The high viscosity water-soluble unit dose detergent composition according to claim 1, further comprising a water-insoluble functional material, wherein the water-insoluble functional material is one of microcapsules, oil droplet essence, petal gel, pearl powder, pearl slurry, pellets, soft beads, or a combination of at least two thereof; the water-insoluble functional substance is added to the A-phase component, or to the B-phase component, or to the A-phase component and the B-phase component, respectively.
5. The high viscosity water-soluble unit dose detergent composition according to claim 1,
The alkaline regulator is one of sodium hydroxide, potassium hydroxide, monoethanolamine and triethanolamine, or the combination of at least two of the above;
The dosage of the carboxyl protecting agent is not zero, and the carboxyl protecting agent is one of citric acid, oxalic acid, tartaric acid, lactic acid, formic acid, acetic acid and sulfamic acid, or the combination of at least two of the citric acid, oxalic acid, tartaric acid, lactic acid, formic acid, acetic acid and sulfamic acid;
the solvent is one of water, ethanol, ethylene glycol, propylene glycol, glycerol, diethylene glycol, dipropylene glycol, polyethylene glycol, polypropylene glycol, dipropylene glycol butyl ether and sorbitol, or a combination of at least two of the two;
the surfactant is one of anionic surfactant, nonionic surfactant and amphoteric surfactant, or the combination of at least two of them.
6. The high viscosity water-soluble unit dose detergent composition according to claim 4,
The phase A component comprises 20 to 59.9 mass percent of surfactant, 10 to 50 mass percent of solvent, 0.1 to 5 mass percent of alkaline regulator and 0.1 to 1.5 mass percent of water-insoluble functional substance;
the phase B component comprises 0.1-20% of surfactant, 10-60% of solvent, 1-25% of polymer thickener and 0-4% of carboxyl protecting agent by mass percent.
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