CN115926896A - High viscosity water soluble unit dose detergent compositions and process for making same - Google Patents
High viscosity water soluble unit dose detergent compositions and process for making same Download PDFInfo
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- 239000003599 detergent Substances 0.000 title claims abstract description 35
- 239000000203 mixture Substances 0.000 title claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 8
- 230000008569 process Effects 0.000 title claims abstract description 6
- 229920000642 polymer Polymers 0.000 claims abstract description 31
- 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 17
- 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
- 239000000126 substance Substances 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000002360 preparation method Methods 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
- 150000001875 compounds Chemical class 0.000 claims description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- -1 acrylic acid/ester compound Chemical class 0.000 claims description 8
- 239000003945 anionic surfactant Substances 0.000 claims description 6
- 239000011324 bead Substances 0.000 claims description 6
- 239000002736 nonionic surfactant 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-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
- 239000002280 amphoteric surfactant Substances 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
- 239000003094 microcapsule Substances 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
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- 230000002209 hydrophobic effect Effects 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000002002 slurry 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
- 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
- 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 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 235000011054 acetic acid Nutrition 0.000 claims description 3
- 239000002775 capsule Substances 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 239000008188 pellet Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000002156 mixing Methods 0.000 abstract description 7
- 239000003607 modifier Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 15
- 239000007788 liquid Substances 0.000 description 10
- 238000005406 washing Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000686 essence Substances 0.000 description 4
- 238000005491 wire drawing Methods 0.000 description 4
- 150000002191 fatty alcohols Chemical class 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- UYTPUPDQBNUYGX-UHFFFAOYSA-N guanine Chemical compound O=C1NC(N)=NC2=C1N=CN2 UYTPUPDQBNUYGX-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000003755 preservative agent Substances 0.000 description 3
- 230000002335 preservative effect Effects 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
- 238000005520 cutting process Methods 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 235000019387 fatty acid methyl ester Nutrition 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
- 238000011068 loading method Methods 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000006187 pill 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
- ATVJXMYDOSMEPO-UHFFFAOYSA-N 3-prop-2-enoxyprop-1-ene Chemical class C=CCOCC=C ATVJXMYDOSMEPO-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 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
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 229940086737 allyl sucrose Drugs 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 230000008859 change Effects 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
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 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
- 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
- 238000009472 formulation Methods 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 229930182470 glycoside Natural products 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
- 239000004615 ingredient Substances 0.000 description 1
- 229940026210 lauramidopropylamine oxide Drugs 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000007858 starting material Substances 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
Abstract
A high viscosity water soluble unit dose detergent composition is disclosed. Having a sachet made from a water-soluble film, the sachet having at least one enclosed chamber enclosing contents therein; the content is formed by blending a phase A component and a phase B 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 thickening agent and a carboxyl protective agent; the polymer type thickener is an emulsion or powdery acrylic acid/ester polymer; and the surfactant is added into the A phase component, or the B phase component, or the A phase component and the B phase component respectively. Its preparing process is also disclosed. The invention can effectively solve the technical problem that the high-viscosity content is difficult to inject in the production process of the water-soluble unit dose detergent.
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 water-soluble unit dose washing products such as washing condensation beads and the like are novel detergents which utilize water-soluble polymer films to wrap contents, and have the advantages of convenient use, attractive appearance, diversified functions and the like, so the water-soluble unit dose washing products occupy a certain share in the detergent markets at home and abroad. According to different application scenes and washing objects, the wrapped contents comprise liquid, powder, particles and even blocky detergents. Due to the limitations of the production equipment and processes, the contents rarely have a high viscosity state. A high viscosity base will give a more concentrated look and feel to the consumer; some water-soluble unit dose detergent products incorporate water-insoluble functional materials (e.g., microcapsules, pearlescents, petals, etc.), and higher system viscosity can reduce the settling rate of the object and help to maintain the stability of the system.
The general manufacturing process for 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 mould, then 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 washing products, the contents of the same chamber are injected in a substantially all disposable manner. During the pouring, if the detergent is a liquid having a relatively high viscosity, there is a possibility of a "stringing" phenomenon occurring above the pouring nozzle and the groove. The "stringing" phenomenon may lead to two negative effects: on one hand, as the wire drawing is required to be broken, the staying time of the liquid injection nozzle can be adjusted and lengthened, and the liquid injection efficiency is reduced; on the other hand, during nozzle dwell, the partial "stringing" does not break and accidentally drip the liquid contents to the film seal site, affecting the seal effect and even causing unit dose product leakage. Therefore, how to prepare a unit dose detergent with high viscosity content is a technical problem 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 said high viscosity water soluble unit dose detergent composition.
In order to achieve the first purpose, the invention adopts the following technical scheme:
a high viscosity water soluble unit dose detergent composition having a sachet made from a water soluble film, the sachet having at least one enclosed chamber within which the contents are enclosed; the content is formed by blending a phase A component and a phase B component; wherein, the phase A component at least comprises 10 to 50 mass percent of solvent and 0.1 to 5 mass percent of alkaline regulator based on the total mass of the encapsulated content; the phase B component at least comprises 10-60% of solvent, 1-25% of polymer thickening agent and 0-4% of carboxyl protective agent by mass percent; the polymer type thickener is an emulsion or powdery acrylic acid/ester polymer; the total mass percentage of the solvent is 20-71%; and the surfactant is added into the phase A component, or the phase B component, or the phase A component and the phase B component respectively in a mass percent of 21-60%.
Preferably, the polymer type thickener is formed by polymerizing an acrylic acid/ester compound serving as a monomer with other hydrophobic compound monomers and/or amphiphilic compound monomers. More preferably, the polymeric thickener has ionizable hydrophilic groups on the molecular chain, and the hydrophilic groups include carboxyl groups.
Preferably, the content has a viscosity of not less than 1000 mPaS and a pH of 6.5 to 8.5.
Further, the water-insoluble functional substance is one of microcapsules, oil drop essence, petal gel, pearl essence, pearl slurry, micro-pills and soft beads, or the combination of at least two of the microcapsules, the oil drop essence, the petal gel, the pearl essence, the pearl slurry, the micro-pills and the soft beads; the water-insoluble functional substance is added into the phase A component, or added into the phase B component, or added into the phase A component and the phase B component respectively.
Preferably, the alkaline regulator is one of sodium hydroxide, potassium hydroxide, monoethanolamine, triethanolamine, or a combination of at least two of them; the dosage of the carboxyl protective agent is not zero, and the carboxyl protective 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, the oxalic acid, the tartaric acid, the lactic acid, the formic acid, the acetic acid and the 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 above; the surfactant is one of an anionic surfactant, a nonionic surfactant and an amphoteric surfactant, or a 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 type thickening agent and 0-4% of carboxyl protective agent in percentage by mass.
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 a phase A component and a phase B component;
2) Injecting the phase A component and the phase B component into a mold cavity for preparing a single capsule in sequence or simultaneously;
3) After the product finished product is prepared, the product finished product is vibrated for 10 to 50 seconds at the frequency of 50 to 300 times/minute with the amplitude of 5 to 20mm, so that the phase A component and the phase B component are completely mixed; or naturally storing to make the phase A component and the phase B component completely mixed.
Preferably, the phase B component is formulated by the steps of:
11 Adding the carboxyl protecting agent into the solvent and adjusting the pH value to be not more than 6.0;
12 Pre-dissolving and dispersing the polymer type thickening agent by using 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.
Preferably, the pH value of the phase A component is 7.5-10.5, and the pH value of the phase B component is 3.0-6.0; the weight ratio of the phase A component to the phase B component is 2; the viscosity of the phase A component is not more than 800mPa & S; the viscosity of the phase B component is not more than 800 mPa.S.
By adopting the technical scheme, the invention can effectively solve the technical problem that high-viscosity contents are difficult to inject in the production process of the water-soluble unit dose detergent; and the high viscosity of the contents can also help the suspension of the water-insoluble functional substances, so that the product is more novel and fashionable in visual appearance.
Detailed Description
The present invention will be further described with reference to the following examples.
In the following examples, the viscosities are the absolute viscosity of a newtonian fluid and the apparent viscosity of a non-newtonian fluid, as measured by a rotational viscometer at 25 ℃. The viscometer speed was fixed at 12 rpm, taking into account the change in apparent viscosity of the non-Newtonian fluid as a function of shear. In order to determine the viscosity status of the contents of an encapsulated unit dose detergent product, the encapsulated and fully reacted unit dose detergent product is manually cut through a sealing film and the contents are poured out, the contents totaling at least 100mL.
The invention divides the content in the unit dose detergent bag 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 twice; 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 can be improved.
The preparation method of the high-viscosity water-soluble unit dose detergent composition comprises the following steps:
1) And respectively preparing a phase A component and a phase B component with low viscosity. 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 comprises 0.1 to 20 percent of surfactant, 10 to 60 percent of solvent, 0 to 4 percent of carboxyl protective agent and 1 to 25 percent of polymer thickening agent.
2) Injecting the phase A component and the phase B component into a mold cavity for preparing a single capsule in sequence or simultaneously;
3) After the finished product is prepared by encapsulating the membrane in bags, carrying out oscillation treatment on the finished product for 10-50 seconds at the amplitude of 5-20mm and the frequency division rate of 50-300 times by using oscillation equipment such as a shaking table, a uniformly mixing device, a vibrating screen and the like; or naturally stored to obtain high viscosity contents.
The viscosity of the above-mentioned phase A component and phase B component should be not more than 800 mPaS, preferably not more than 600 mPaS. The viscosity of the content of the finished product is not less than 1000 mPaS, and the better viscosity range is 5000-30000 mPaS.
The polymer type thickener is emulsion or powder acrylic acid/ester polymer, which is prepared from acrylic acid/ester compound as monomer (one) and other hydrophobic compound monomer and/or hydrophobic compoundThe amphiphilic compound monomer is polymerized. Other monomers other than the (acrylate) compound include: allyl ether compounds, allyl sucrose, allyl pentaerythritol, alkyl methacrylates, alkanol acrylates, styrene, N' -methylenebisacrylamide. Further, the polymeric thickener may be selected from Lumboyants
Aqua SF-1 Polymer、/>
ETD 2020 Polymer、/>
L-10 Polymer、/>
L-20 Polymer, and Volarest, poa TM And FL. Further, the acrylic acid/ester-based 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 Using the solvent obtained in the step 11) to pre-dissolve and disperse the polymer type thickening agent, and uniformly stirring; 13 Add the remaining components to obtain phase B component.
The pH value of the phase A component is preferably controlled to be 7.5-10.5, the pH value of the phase B component is controlled to be 3.0-6.0, the weight ratio of the two phases is 2-8, and the more preferable weight ratio is 4.
The pH value of the finished product is preferably between 6.5 and 8.5 after the phase A component and the phase B component are fully mixed.
The water-insoluble functional substance in the phase A component is at least one of microcapsule, oil drop essence, petal gel, pearl essence, pearl slurry, pellet 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 generate high viscosity, which affects normal production, it is desirable to add a suitable amount of a carboxyl group protecting agent when formulating the phase B component to ensure that the carboxyl groups do not react with other compounds in the phase B component before mixing with the phase a component. The carboxyl protective agent is one or more of citric acid, oxalic acid, tartaric acid, lactic acid, formic acid, acetic acid and sulfamic acid.
The solvent of 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 a mixture thereof.
The surfactant in the above-mentioned phase a component and phase B component comprises 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 alkyl benzene 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 glucoside, fatty acid methyl ester ethoxylate and grease ethoxylate. The zwitterionic surfactant may be selected from one or more of the 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 preservative can be added into the product content.
It should be noted that the sachet 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 chamber of the present invention is composed of two sub-chambers and a communicating cavity communicating the two sub-chambers. In the preparation process, the A-phase component and the B-phase component can be simultaneously and respectively injected into one sub-chamber, and the blending is realized through the communicating chamber.
Examples 1 to 4
Examples 1-4 use thickeners of
Aqua SF-1. The ingredient ratios and related performance parameters of the products of the four examples and the three comparative examples are shown in Table 1.
The specific preparation method for the four examples and the three comparative examples is as follows:
1. preparing a phase A component: adding a solvent and an alkaline regulator into a reaction kettle, and uniformly stirring; and then adding an anionic surfactant, uniformly stirring, then adding a nonionic surfactant and an amphoteric surfactant, adjusting the pH to meet the regulation, adding a water-insoluble functional substance and a preservative, and finally measuring the final pH and viscosity.
Preparing a phase B component: adjusting the pH value of propylene glycol as a solvent to be below 6.0 by using a carboxyl protective agent, then adding a polymer type thickening agent, dispersing and dissolving the polymer type thickening agent, adding the rest components after uniformly stirring, and finally measuring the final pH value and viscosity.
The phase B composition of comparative example 3 was prepared as follows: the preparation method comprises the steps of uniformly mixing a solvent propylene glycol and a polymer type thickening agent, adding other components except the carboxyl protective agent, uniformly stirring, and finally adding the carboxyl protective agent.
2. Loading on a machine for film sealing: and deforming the water-soluble film by utilizing vacuum and adsorbing the water-soluble film on the inner side of the groove of the mold, then injecting the phase A component and the phase B component into the same mold cavity of the mold in sequence through a nozzle, sealing the film and cutting the film into single finished products. Placing each finished product on a shaking table, and shaking for 10-50 seconds at an amplitude of 5-20mm and a frequency division rate of 50-300 times.
TABLE 1
As can be seen from table 1, the difference between example 1 and comparative example 1 is whether or not a polymeric thickener is added to the phase B component. From the petal states of the two, the phase B component of comparative example 1 did not have the effect of stabilizing the petals because no polymeric thickener was added, and the product settled after standing at room temperature for one day. Whereas example 1 had a higher viscosity and could maintain a good appearance for a long period of time.
Comparative example 2 is a sample with the phase a components being not made alkaline, and comparative example 3 is a sample with the phase B components not having the carboxyl group protecting agent added first. From the encapsulated state of comparative example 2, for a product in which the pH is not adjusted to a reasonable range, even if the phase a component and the phase B component are injected into the unit dose cavity sequentially according to the preparation method, the phenomena of liquid leakage, wire drawing and the like occur in the production process of the formula, and the normal production is affected. In comparative example 3, although the pH of the late phase B component was also adjusted to 6.0 or less, since the carboxyl group was reacted with other compounds without first adding the carboxyl group protecting agent, the high viscosity phase B was formed, and then the polymeric thickener was directly flocculated into masses even though the carboxyl group protecting agent was added. Therefore, the composition of the present invention requires a strictly defined production process, otherwise even the same combination, pH, would result in a production failure.
Example 2, example 3 and example 4 are different weight ratios of phase a component to phase B component of the unit dose composition. From the results, it can be seen that the weight ratio between the phase A and the phase B of the composition is not limited, but the reaction ratio is designed to be within the range after the phase A and the phase B are added in proportion, so that the unit dose detergent product can be normally encapsulated and has the effect of stabilizing petals.
Furthermore, in example 4, the total surfactant content was only 21%, indicating that the present invention can be implemented in either a normal or concentrated unit dose detergent.
Examples 5 to 6
Examples 5 to 6 use thickeners in the form of powders
ETD 2020 Polymer. The product composition ratios and related performance parameters of the two examples and the three comparative examples are shown in table 2.
The specific preparation method of the two examples and the three comparative examples is as follows:
1. preparing a phase A component: adding a solvent and an alkaline regulator into a reaction kettle, and uniformly stirring; and then adding an anionic surfactant, uniformly stirring, then adding a nonionic surfactant and an amphoteric surfactant, adjusting the pH to meet the regulation, adding a water-insoluble functional substance and a preservative, and finally measuring the final pH and viscosity.
Preparing a phase B component: adjusting the pH value of the pure water to be below 6.0 by using a carboxyl protective agent; then spreading the powdery polymer type thickening agent in the liquid, standing for wetting, and uniformly stirring. Finally, the remaining components were added and the final pH and viscosity were determined.
2. Loading on a machine for film sealing: and deforming the water-soluble film by utilizing vacuum and adsorbing the water-soluble film on the inner side of the groove of the mold, then injecting the phase A component and the phase B component into the same mold cavity of the mold in sequence through a nozzle, sealing the film and cutting the film into single finished products. Placing each finished product on a shaking bed, and shaking for 10-50 seconds at an amplitude of 5-20mm and a frequency division rate of 50-300 times.
TABLE 2
From the states of the water-insoluble functional materials of example 5 and comparative example 4, by the method for preparing the high viscosity water-soluble unit dose detergent described in the present invention,
ETD 2020 Polymer can also be used in unit dose products and acts to thicken and suspend particles. />
From the analysis of example 6 and comparative example 5, in comparative example 5, the pH control of the A phase and the B phase of the composition is in the range, but since the neutralization reaction of the two phases is not properly adjusted after the addition of the composition according to the proportion, the encapsulation is affected, and the preparation is not normal, the limitation of the pH and the reaction ratio of the two phases is required in the invention, and simultaneously, the effect of the invention can not be achieved by simply adjusting the pH. Comparative example 6 the phase a and the phase B were mixed to prepare the same phase, which was then filled and encapsulated. However, the viscosity of the two phases after mixing is too high, and the phenomenon of 'wire drawing' is generated during liquid injection of the liquid injection nozzle, so that the encapsulation has problems, which shows that the invention can effectively avoid the phenomenon of 'wire drawing' in production and obtain a high-viscosity unit dose washing product.
Examples 7 to 9
In example 7, since the component of phase B contains only solvent, thickener and a small amount of surfactant, the present invention can be achieved even without adding a carboxyl group protecting agent,
ETD 2020 Polymer can also be used in unit dose products and acts to thicken and suspend particles. In examples 8 and 9, the addition of 8% of a C8-C14 alkyl glycoside makes the starting material more basic, so that a higher amount of acidic protecting agent must be added to ensure that the viscosity remains low until the A and B phases are mixed. In example 9, the invention was also realized when the surfactant content in phase A reached 40% or more and the surfactant ratio in the formulation was adjusted to reduce the viscosity to 800 mP.S or less. />
Claims (10)
1. A high viscosity water soluble unit dose detergent composition having a sachet made from a water soluble film, the sachet having at least one enclosed chamber enclosing contents, characterised in that the contents are blended from a phase a component 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 by mass percent;
the phase B component at least comprises 10-60% of solvent, 1-25% of polymer thickening agent and 0-4% of carboxyl protective agent by mass percent; the polymer type thickener is an emulsion or powdery acrylic acid/ester polymer;
the total mass percentage of the solvent is 20-71%;
the detergent also comprises 21-60% of surfactant by mass, wherein the surfactant is added into the A phase component, or added into the B phase component, or added into the A phase component and the B phase component respectively.
2. The high viscosity water soluble unit dose detergent composition according to claim 1, wherein said polymeric thickener is polymerized with other hydrophobic compound monomer and/or amphiphilic compound monomer using acrylic acid/ester compound as monomer.
3. The high viscosity water soluble unit dose detergent composition according to claim 2, wherein said polymeric thickener has ionizable hydrophilic groups in the molecular chain, said hydrophilic groups comprising carboxyl groups.
4. The high viscosity water soluble unit dose detergent composition according to claim 1, wherein the viscosity of the contents is not less than 1000 mPa-S, and the pH is 6.5 to 8.5.
5. The high viscosity water soluble unit dose detergent composition according to claim 1, further comprising a water insoluble functional substance, wherein the water insoluble functional substance is one of a microcapsule, an oil droplet essence, a petal gel, a pearl powder, a pearl slurry, a pellet, a soft bead, or a combination of at least two thereof; the water-insoluble functional substance is added into the phase A component, or added into the phase B component, or added into the phase A component and the phase B component respectively.
6. 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 sodium hydroxide, the potassium hydroxide, the monoethanolamine and the triethanolamine;
the dosage of the carboxyl protective agent is not zero, and the carboxyl protective 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, the oxalic acid, the tartaric acid, the lactic acid, the formic acid, the acetic acid and the 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 above;
the surfactant is one of an anionic surfactant, a nonionic surfactant and an amphoteric surfactant, or a combination of at least two of them.
7. The high viscosity water soluble unit dose detergent composition according to claim 5,
the phase A component comprises 20-59.9% of surfactant, 10-50% of solvent, 0.1-5% of alkaline regulator and 0.1-1.5% of water-insoluble functional substance by mass percentage;
the phase B component comprises 0.1-20% of surfactant, 10-60% of solvent, 1-25% of polymer type thickening agent and 0-4% of carboxyl protective agent in percentage by mass.
8. A process for the preparation of a high viscosity water soluble unit dose detergent composition as claimed in any of claims 1 to 7 consisting of the steps of:
1) Respectively preparing a phase A component and a phase B component;
2) Injecting the phase A component and the phase B component into a mold cavity for preparing a single capsule in sequence or simultaneously;
3) After the product finished product is prepared, the product finished product is vibrated for 10 to 50 seconds at the frequency of 50 to 300 times/minute with the amplitude of 5 to 20mm, so that the phase A component and the phase B component are completely mixed; or naturally storing to make the phase A component and the phase B component completely mixed.
9. The process of claim 8, wherein the phase B component is formulated by:
11 Adding the carboxyl protecting agent into the solvent and adjusting the pH value to be not more than 6.0;
12 Pre-dissolving and dispersing the polymer type thickening agent by using the solvent obtained in the step 11), and uniformly stirring;
13 Then adding the remaining components to obtain a B phase component;
the pH of the polymeric thickener is no greater than 6.5.
10. The method according to claim 8,
the pH value of the phase A component is 7.5-10.5, and the pH value of the phase B component is 3.0-6.0; the weight ratio of the phase A component to the phase B component is 2;
the viscosity of the phase A component is not more than 800mPa & S; the viscosity of the phase B component is not more than 800 mPa.S.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1814722A (en) * | 2006-01-16 | 2006-08-09 | 张宏格 | Liquid detergent viscosity-increasing agent |
| US20080051314A1 (en) * | 2006-08-24 | 2008-02-28 | Kimberly-Clark Worldwide, Inc. | Liquid cleanser formulation with suspending and foaming capabilities |
| CN102264886A (en) * | 2008-12-29 | 2011-11-30 | 埃科莱布有限公司 | highly viscous detergent emulsion |
| CN105694322A (en) * | 2016-01-20 | 2016-06-22 | 广州立白企业集团有限公司 | Water-soluble thin film with good water dissolving performance and small bag prepared from water-soluble thin film |
| CN114774210A (en) * | 2021-05-26 | 2022-07-22 | 郭建华 | Low temperature stable unit dose detergent compositions |
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2022
- 2022-11-02 CN CN202211361275.9A patent/CN115926896A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1814722A (en) * | 2006-01-16 | 2006-08-09 | 张宏格 | Liquid detergent viscosity-increasing agent |
| US20080051314A1 (en) * | 2006-08-24 | 2008-02-28 | Kimberly-Clark Worldwide, Inc. | Liquid cleanser formulation with suspending and foaming capabilities |
| CN102264886A (en) * | 2008-12-29 | 2011-11-30 | 埃科莱布有限公司 | highly viscous detergent emulsion |
| CN105694322A (en) * | 2016-01-20 | 2016-06-22 | 广州立白企业集团有限公司 | Water-soluble thin film with good water dissolving performance and small bag prepared from water-soluble thin film |
| CN114774210A (en) * | 2021-05-26 | 2022-07-22 | 郭建华 | Low temperature stable unit dose detergent compositions |
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