CN115873667B - Capsule type concentrated detergent and preparation method thereof - Google Patents
Capsule type concentrated detergent and preparation method thereof Download PDFInfo
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- CN115873667B CN115873667B CN202211500985.5A CN202211500985A CN115873667B CN 115873667 B CN115873667 B CN 115873667B CN 202211500985 A CN202211500985 A CN 202211500985A CN 115873667 B CN115873667 B CN 115873667B
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- 239000003599 detergent Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000002775 capsule Substances 0.000 title claims abstract description 32
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 75
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229920002545 silicone oil Polymers 0.000 claims abstract description 39
- 239000002131 composite material Substances 0.000 claims abstract description 37
- 239000000839 emulsion Substances 0.000 claims abstract description 34
- 239000000835 fiber Substances 0.000 claims abstract description 30
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 26
- 229920001661 Chitosan Polymers 0.000 claims abstract description 26
- 239000001110 calcium chloride Substances 0.000 claims abstract description 26
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 26
- -1 alkyl glycoside Chemical class 0.000 claims abstract description 19
- 108090000790 Enzymes Proteins 0.000 claims abstract description 18
- 102000004190 Enzymes Human genes 0.000 claims abstract description 18
- 108010010803 Gelatin Proteins 0.000 claims abstract description 18
- 229920000159 gelatin Polymers 0.000 claims abstract description 18
- 239000008273 gelatin Substances 0.000 claims abstract description 18
- 235000019322 gelatine Nutrition 0.000 claims abstract description 18
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 18
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 14
- 229930182470 glycoside Natural products 0.000 claims abstract description 13
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 13
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 13
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 11
- WJRBRSLFGCUECM-UHFFFAOYSA-N hydantoin Chemical compound O=C1CNC(=O)N1 WJRBRSLFGCUECM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229940091173 hydantoin Drugs 0.000 claims abstract description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 11
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 11
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 89
- 239000000243 solution Substances 0.000 claims description 62
- 239000003094 microcapsule Substances 0.000 claims description 53
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 42
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 239000002134 carbon nanofiber Substances 0.000 claims description 27
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 27
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 19
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 17
- 229940088598 enzyme Drugs 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 238000009987 spinning Methods 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 229920000570 polyether Polymers 0.000 claims description 14
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000008394 flocculating agent Substances 0.000 claims description 10
- 235000010323 ascorbic acid Nutrition 0.000 claims description 9
- 229960005070 ascorbic acid Drugs 0.000 claims description 9
- 239000011668 ascorbic acid Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 238000010041 electrostatic spinning Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 5
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005538 encapsulation Methods 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 5
- 229940057995 liquid paraffin Drugs 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 235000010413 sodium alginate Nutrition 0.000 claims description 5
- 239000000661 sodium alginate Substances 0.000 claims description 5
- 229940005550 sodium alginate Drugs 0.000 claims description 5
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 5
- 230000008023 solidification Effects 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 3
- 108010067770 Endopeptidase K Proteins 0.000 claims description 3
- 108090000526 Papain Proteins 0.000 claims description 3
- 239000004365 Protease Substances 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 229940055729 papain Drugs 0.000 claims description 3
- 235000019834 papain Nutrition 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 3
- 239000004299 sodium benzoate Substances 0.000 claims description 3
- 235000010234 sodium benzoate Nutrition 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 13
- 238000003860 storage Methods 0.000 abstract description 5
- 238000011010 flushing procedure Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000463 material Substances 0.000 description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 6
- 239000013543 active substance Substances 0.000 description 5
- 239000002518 antifoaming agent Substances 0.000 description 3
- 238000005202 decontamination Methods 0.000 description 3
- 230000003588 decontaminative effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004851 dishwashing Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Detergent Compositions (AREA)
Abstract
The invention relates to the technical field of articles for daily use, in particular to a capsule type super-concentrated detergent and a preparation method thereof, wherein the capsule type super-concentrated detergent comprises the following components in parts by weight: 25-40 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 10-20 parts of alkyl glycoside, 8-15 parts of modified silicone oil, 15-30 parts of sodium dodecyl sulfate, 0.5-3 parts of citric acid, 0.3-1 part of enzyme, 0.05-0.1 part of hydantoin, 6-15 parts of auxiliary agent, 80-120 parts of water/oil emulsion, 50-80 parts of calcium chloride-containing chitosan solution, 50-70 parts of gelatin solution, 1-3 parts of flocculant, 3-7 parts of composite fiber and 2-5 parts of glutaraldehyde. The capsule type super-concentrated detergent disclosed by the invention has a very strong emulsifying and decontaminating effect, can be used for rapidly and efficiently dissolving and emulsifying oil stains, harmful substances and dispersing and suspending, and can be separated from the surface of tableware by flushing with clear water, so that the effect of efficiently cleaning the tableware is achieved, the stability is good, the storage period is long, and the cost of transportation and storage is reduced.
Description
Technical Field
The invention relates to the technical field of articles for daily use, in particular to a capsule type concentrated detergent and a preparation method thereof.
Background
With the development of the integration and trade globalization of world economy, cultural background, technical level and environmental protection regulations are becoming three major drivers of globalization development of washing products, the global washing products will tend to be diversified, but the products which are energy-saving, water-saving, efficient, mild, convenient to use and meet the requirements of safety and environmental protection will be the main stream direction of the development of the current and future washing products. The detergent is a product which is commonly used in families and used for cleaning dirt and greasy dirt, and the performance of the product affects the health of human beings. Therefore, the detergent is required to have the characteristics of safety, environment protection, clean and mild, soft and fine foam and rapid oil decomposition, so that the aims of rapid decontamination, sterilization, effective and thorough cleaning and no residue are fulfilled.
For example, the invention patent with publication number CN102994242a discloses a super concentrated detergent powder, which is mainly prepared by mixing the following components in percentage by weight: 82-97% of solid surfactant, 1-12% of builder and 0.1-8% of thickener; the super-concentrated detergent powder contains no water, has a mild formula, has super-strong detergency, and has a concentration multiple of at least 5 times that of the common detergent; however, the solid surfactant in the detergent has poor wetting spreadability, cannot realize complete infiltration of oil stains, and causes poor permeability of the detergent to the interface between the tableware substrate and the oil stains, so that the cleaning effect is affected, a large amount of detergent is often required to be used for achieving a satisfactory cleaning effect, a large amount of foam is generated along with the increase of the use amount of the detergent, the problem of detergent residue is easy to generate, and a large amount of water is required to be consumed for thoroughly cleaning, so that the cost for cleaning dirt and oil stains is increased.
Disclosure of Invention
The invention aims to provide a capsule type concentrated detergent and a preparation method thereof.
In order to achieve the above purpose, the present invention provides the following technical solutions:
A capsule type concentrated detergent comprises the following components in parts by weight: 25-40 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 10-20 parts of alkyl glycoside, 8-15 parts of modified silicone oil, 15-30 parts of sodium dodecyl sulfate, 0.5-3 parts of citric acid, 0.3-1 part of enzyme, 0.05-0.1 part of hydantoin, 6-15 parts of auxiliary agent, 80-120 parts of water/oil emulsion, 50-80 parts of calcium chloride-containing chitosan solution, 50-70 parts of gelatin solution, 1-3 parts of flocculant, 3-7 parts of composite fiber and 2-5 parts of glutaraldehyde.
As a further preferable scheme of the invention, the enzyme is prepared from proteinase K and papain according to a mass ratio of 1: (1-3);
The auxiliary agent is prepared from urea, ethylenediamine tetraacetic acid, salt, sodium benzoate and trisodium citrate according to the mass ratio of 1: (0.2-0.6): (0.6-1.3): (1-3): (0.1-0.7);
the concentration of the gelatin solution is 5-8wt%;
the flocculant is prepared from sodium sulfate and ammonium sulfate according to a mass ratio of 1: (1.0-1.5).
As a further preferable embodiment of the present invention, the preparation method of the water/oil type emulsion is as follows:
Emulsifying 5-10mL of sodium alginate solution with concentration of 2-6wt% into 30-50mL of liquid paraffin containing 5-8wt% span-80, and magnetically stirring for 10-30 min;
The preparation method of the chitosan solution containing calcium chloride comprises the following steps:
Adding acetic acid into 10-20mL distilled water according to the proportion of 1-3wt%, uniformly mixing, adding 3-7g chitosan, fully stirring and dissolving, adding 0.6-1.2g calcium chloride, and fully stirring.
As a further preferable scheme of the invention, the preparation method of the modified silicone oil comprises the following steps:
Dissolving dry chloroplatinic acid in distilled isopropanol, fully stirring, standing overnight to obtain a product A, adding allyl polyether and hydrogen-containing silicone oil into a container, introducing enough nitrogen to exhaust air, heating to 60-80 ℃, then dropwise adding the product A, stirring for reacting for 4-6h, and after the reaction is finished, distilling under reduced pressure to remove low-boiling substances to obtain the modified silicone oil.
As a further preferable mode of the invention, the dosage proportion of the chloroplatinic acid and the isopropanol is (1-3) g: (60-100) mL;
the mass ratio of the allyl polyether to the hydrogen-containing silicone oil to the product A is (10-15): (5-8): (0.1-0.5).
As a further preferable scheme of the invention, the hydrogen content of the hydrogen-containing silicone oil is 0.18-0.75%, and the viscosity is 54-152mm 2/s;
The molecular weight of the allyl polyether is 300-600.
A preparation method of a capsule type concentrated detergent specifically comprises the following steps:
1) Weighing the components according to the parts by weight, adding the fatty alcohol polyoxyethylene ether sodium sulfate, the alkyl glycoside and the modified silicone oil into the water/oil type emulsion, fully stirring, dropwise adding the calcium chloride-containing chitosan solution under stirring, continuously stirring after the dropwise adding, demulsifying and layering with isopropanol, and repeatedly washing with distilled water while vacuum suction filtering to obtain a microcapsule A;
2) Adding enzyme into water/oil emulsion, stirring thoroughly, dropwise adding calcium chloride-containing chitosan solution under stirring, stirring continuously after dropwise adding, demulsifying and layering with isopropanol, vacuum filtering, and washing with distilled water repeatedly to obtain microcapsule B;
3) Adding sodium dodecyl sulfonate, citric acid, hydantoin and an auxiliary agent into a gelatin solution, fully stirring at 35-40 ℃, adding a microcapsule A and a microcapsule B to obtain emulsion, adding a flocculating agent into the emulsion under stirring, dividing the flocculating agent into 5-8 equal parts, adding one part every 5-10min, adding a composite fiber into the mixture after encapsulation, and keeping stirring and maintaining the temperature at 35-40 ℃ in the whole process to obtain microcapsule particles;
4) And (3) placing the microcapsules in ice water for cooling, stirring until the microcapsules are completely condensed, adding glutaraldehyde for solidification for 2-4 hours, standing the microcapsule solution, precipitating, pouring out the upper liquid and recovering the flocculant, and freeze-drying the microcapsules at the bottom layer to obtain the required capsule type concentrated detergent.
As a further preferable embodiment of the present invention, the preparation method of the composite fiber is as follows:
1) Carrying out electrostatic spinning on spinning solution formed by mixing polyacrylonitrile and N, N-dimethylformamide, drying a spinning product, placing the spinning product in a tubular furnace, carrying out heat treatment for 1-3h at 300-350 ℃ in air atmosphere, and then carrying out heat treatment for 1-3h at 800-860 ℃ in nitrogen atmosphere to obtain carbon nanofibers;
2) Immersing the carbon nanofiber into a silver-ammonia solution composed of ethanol, silver nitrate and ammonia water, immersing for 5-10h, taking out, putting into a polyvinylpyrrolidone ethanol solution, and stirring and reacting for 3-5h at 70-76 ℃ to obtain the pretreated carbon nanofiber;
3) Immersing the pretreated carbon nanofiber into a silver nitrate and citric acid composite aqueous solution, dropwise adding an ascorbic acid aqueous solution, continuously reacting for 4-9 hours under ultrasonic and stirring, repeatedly washing with ultrapure water after the reaction is finished, and drying to obtain the composite fiber.
As a further preferable mode of the invention, the mass ratio of the polyacrylonitrile to the N, N-dimethylformamide is (5-8): (92-95);
The electrostatic spinning voltage is 15-20kV, the receiving distance is 10-15cm, and the flow rate is 0.5-1.5mL/h;
The dosage proportion of the carbon nanofiber, ethanol, silver nitrate, ammonia water and polyvinylpyrrolidone ethanol solution is (3-8) g: (40-50) mL: (0.4-0.9) g: (3-6) mL: (50-70) mL;
the concentration of the polyvinylpyrrolidone ethanol solution is 20-30mg/mL.
As a further preferable scheme of the invention, the dosage proportion of the pretreated carbon nanofiber, the silver nitrate and citric acid composite aqueous solution and the ascorbic acid aqueous solution is (2-5) g: (70-100) mL: (20-28) mL;
The concentration of the silver nitrate and citric acid composite aqueous solution is 6.5-7.0mg/mL, wherein the molar ratio of the silver nitrate to the citric acid is 1: (1.0-1.2);
The concentration of the ascorbic acid aqueous solution is 10-15mg/mL.
Compared with the prior art, the invention has the beneficial effects that:
In the invention, an emulsification method is adopted, active agent components of sodium fatty alcohol polyoxyethylene ether sulfate, alkyl glycoside and modified silicone oil, and enzyme are respectively used as core materials to prepare microcapsules, and the raw materials of different components are respectively prepared into the microcapsules, so that the effect of separating the components can be achieved, and the influence on chemical properties after the components are mixed is avoided, thereby influencing the cleaning effect of subsequent use; the active agent components of the fatty alcohol polyoxyethylene ether sodium sulfate, the alkyl glycoside and the modified silicone oil have strong emulsifying and decontaminating effects, can quickly and efficiently dissolve and emulsify oily stains, harmful substances and disperse and suspend, and can be separated from the surface of tableware by washing with clear water, so that the effect of efficiently cleaning the tableware is achieved; in addition, the modified silicone oil is obtained by modifying the silicone oil by adopting polyether substances, wherein polyether is a hydrophilic group, methyl groups on a siloxane chain provide hydrophobic groups, and molecules in water are arranged on an air/water interface in a comb-shaped structure, so that the surface of the water can be tightly covered, water molecules are prevented from penetrating into a surfactant layer of a gas-liquid interface, the surface tension of the water is effectively reduced, the water and oil stains can be uniformly and stably mixed together, and the oil stains can be taken away by the water, so that a better decontamination effect is achieved; the modified silicone oil can be wetted and spread on the low-energy hydrophobic surface, has good spreadability, can realize complete infiltration of oil stains, promotes infiltration of the detergent to the interface between the tableware matrix and the oil stains, and emulsifies, solubilizes and disperses the oil stains so as to be separated from the tableware matrix and dispersed or emulsified in water, thereby further improving the decontamination effect and improving the cleaning cleanliness.
In the invention, gelatin is used as a wall material, and the microcapsule A containing active agent components and the microcapsule B containing enzyme are embedded, so that the capsule type concentrated detergent is obtained, the gelatin can be used as the wall material to play an isolating role, and the components contained in the gelatin are prevented from being in contact with the outside to deteriorate, so that the stability and the storage convenience of the concentrated detergent are improved; in order to improve the strength of the wall material and avoid wall material rupture caused by rapid stirring in the preparation process of the capsule type concentrated detergent, in the invention, composite fibers are added in the wall material, the composite fibers take carbon nanofibers obtained by polyacrylonitrile spinning carbonization as a matrix, nano sheets are constructed on the carbon nanofibers in situ through a two-step chemical synthesis method, and the formed nano sheets form connection sites through mutual embedding and stacking, so that the composite fibers can be better constructed to form a reticular support structure, and the strength of the wall material is improved, so that the wall material rupture phenomenon cannot occur in the preparation process of the capsule type concentrated detergent; and when the capsule-type concentrated detergent is used, gelatin in the wall material can be dissolved in hot water to expose the composite fiber, and as a large number of nano sheets are arranged on the surface of the composite fiber, the surface of the composite fiber is rough, and people can contact and rub the microcapsule A and the microcapsule B contained in the composite fiber under the wiping action when cleaning tableware, so that the rupture of the wall material of the microcapsule A and the microcapsule B is facilitated to be quickened, the outflow of active agent components and enzymes is promoted, the removal speed of greasy dirt is improved, and the cleaning efficiency is improved.
The capsule type concentrated detergent disclosed by the invention has a very strong emulsifying and decontaminating effect, can be used for rapidly and efficiently dissolving and emulsifying oil stains, harmful substances and dispersing and suspending, and can be separated from the surface of tableware by flushing with clear water, so that the effect of efficiently cleaning the tableware is achieved, the stability is good, the storage period is long, and the cost of transportation and storage is reduced.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the embodiment of the invention, the enzyme is prepared from proteinase K and papain according to the mass ratio of 1:2, composing;
the auxiliary agent comprises urea, ethylenediamine tetraacetic acid, salt, sodium benzoate and trisodium citrate according to the mass ratio of 1:0.2:0.6:1: 0.1;
The concentration of the gelatin solution was 5wt%;
The flocculant is prepared from sodium sulfate and ammonium sulfate according to a mass ratio of 1: 1.5.
Example 1
The capsule type concentrated detergent is characterized by comprising the following components in parts by weight: 25 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 10 parts of alkyl glycoside, 8 parts of modified silicone oil, 15 parts of sodium dodecyl sulfate, 0.5 part of citric acid, 0.3 part of enzyme, 0.05 part of hydantoin, 6 parts of auxiliary agent, 80 parts of water/oil emulsion, 50 parts of calcium chloride-containing chitosan solution, 50 parts of gelatin solution, 1 part of flocculant, 3 parts of composite fiber and2 parts of glutaraldehyde;
the preparation method of the water/oil type emulsion comprises the following steps:
Emulsifying 5mL of sodium alginate solution with the concentration of 2wt% into 30mL of liquid paraffin containing 5wt% span-80, and magnetically stirring for 10 min;
the preparation method of the chitosan solution containing calcium chloride comprises the following steps:
taking 10mL of distilled water, adding acetic acid according to the proportion of 1wt%, uniformly mixing, adding 3g of chitosan, fully stirring and dissolving, adding 0.6g of calcium chloride, and fully stirring;
the preparation method of the modified silicone oil comprises the following steps:
Dissolving 1g of dry chloroplatinic acid in 60mL of distilled isopropanol, fully stirring, standing overnight to obtain a product A, adding 10g allyl polyether and 5g hydrogen-containing silicone oil into a container, introducing enough nitrogen to exhaust air, heating to 60 ℃, dropwise adding 0.1g of the product A, stirring at 60r/min for reaction for 4 hours, and distilling under reduced pressure to remove low-boiling substances after the reaction is finished to obtain modified silicone oil, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.18%, the viscosity is 152mm 2/s, and the molecular weight of the allyl polyether is 300.
The preparation method of the composite fiber comprises the following steps:
1) Polyacrylonitrile and N, N-dimethylformamide are mixed according to a mass ratio of 5:95, fully stirring at room temperature until the spinning solution is transparent and uniform, carrying out electrostatic spinning on the formed spinning solution, wherein the voltage is 15kV, the receiving distance is 10cm, the flow rate is 0.5mL/h, drying a product obtained by spinning, placing the product in a tubular furnace, carrying out heat treatment for 1h at 300 ℃ in air atmosphere, and then carrying out heat treatment for 1h at 800 ℃ in nitrogen atmosphere to obtain carbon nanofibers;
2) Immersing 3g of carbon nanofiber into a silver-ammonia solution consisting of 40mL of ethanol, 0.4g of silver nitrate and 3mL of ammonia water, taking out after immersing for 5 hours, putting into 50mL of polyvinylpyrrolidone ethanol solution with the concentration of 20mg/mL, and reacting for 3 hours at 70 ℃ and 50r/min to obtain pretreated carbon nanofiber;
3) 2g of the pretreated carbon nanofiber is immersed in 70mL of a composite aqueous solution of silver nitrate and citric acid, wherein the molar ratio of the silver nitrate to the citric acid is 1:1, then dropwise adding 20mL of 10mg/mL ascorbic acid aqueous solution, continuously reacting for 4 hours at 150W and 100r/min, repeatedly washing with ultrapure water after the reaction is finished, and drying to obtain the composite fiber.
A preparation method of a capsule type concentrated detergent specifically comprises the following steps:
1) Weighing the components according to the parts by weight, firstly adding sodium fatty alcohol polyoxyethylene ether sulfate, alkyl glycoside and modified silicone oil into a half amount of water/oil emulsion, stirring for 20min at 500r/min, then dropwise adding a half amount of calcium chloride-containing chitosan solution under stirring, continuing stirring for 30min after the dropwise adding, then demulsifying and layering with isopropanol, and repeatedly washing with distilled water while vacuum filtration to obtain a microcapsule A;
2) Adding enzyme into the rest half of water/oil emulsion, stirring for 20min at 500r/min, then dropwise adding the rest half of chitosan solution containing calcium chloride under stirring, continuing stirring for 30min after dropwise adding, then demulsifying and layering with isopropanol, vacuum filtering, and repeatedly washing with distilled water to obtain microcapsule B;
3) Adding sodium dodecyl sulfonate, citric acid, hydantoin and an auxiliary agent into a gelatin solution, stirring at the temperature of 35 ℃ for 20min at the speed of 1000r/min, then adding a microcapsule A and a microcapsule B, stirring at the temperature of 100r/min for 10min to obtain an emulsion, adding a flocculating agent into the emulsion under the stirring at the speed of 300r/min, dividing the flocculating agent into 5 equal parts, adding one part every 5min, adding a composite fiber into the emulsion after the mixture is encapsulated, continuing stirring for 30min, and dropwise adding n-butanol as an antifoaming agent for defoaming in the encapsulation process, wherein the whole process keeps stirring and maintains the temperature at 35 ℃ to obtain microcapsule particles;
4) And (3) placing the microcapsules in ice water for cooling, stirring at 130r/min until the microcapsules are completely condensed, adding glutaraldehyde for solidification for 2 hours, standing the microcapsule solution, precipitating, pouring out the upper liquid and recovering the flocculant, and freeze-drying the microcapsules at the bottom layer to obtain the required capsule type concentrated detergent.
Example 2
The capsule type concentrated detergent is characterized by comprising the following components in parts by weight: 35 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 15 parts of alkyl glycoside, 12 parts of modified silicone oil, 25 parts of sodium dodecyl sulfate, 1.5 parts of citric acid, 0.8 part of enzyme, 0.08 part of hydantoin, 10 parts of auxiliary agent, 100 parts of water/oil emulsion, 70 parts of calcium chloride-containing chitosan solution, 60 parts of gelatin solution, 2 parts of flocculant, 5 parts of composite fiber and 3 parts of glutaraldehyde;
the preparation method of the water/oil type emulsion comprises the following steps:
Emulsifying 7mL of sodium alginate solution with concentration of 5wt% into 40mL of liquid paraffin containing 7wt% span-80, and magnetically stirring for 10-30 min;
the preparation method of the chitosan solution containing calcium chloride comprises the following steps:
15mL of distilled water is taken, acetic acid is added according to the proportion of 2 weight percent, 5g of chitosan is added after uniform mixing, 0.9g of calcium chloride is added after full stirring and dissolution, and the preparation is completed after full stirring;
the preparation method of the modified silicone oil comprises the following steps:
Dissolving 2g of dry chloroplatinic acid in 80mL of distilled isopropanol, fully stirring, standing overnight to obtain a product A, adding 13g allyl polyether and 6g hydrogen-containing silicone oil into a container, introducing enough nitrogen to exhaust air, heating to 70 ℃, dropwise adding 0.3g of the product A, stirring at 80r/min for reaction for 5h, and distilling under reduced pressure to remove low-boiling substances after the reaction is finished to obtain modified silicone oil, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.36%, the viscosity is 116mm 2/s, and the molecular weight of the allyl polyether is 400.
The preparation method of the composite fiber comprises the following steps:
1) Polyacrylonitrile and N, N-dimethylformamide are mixed according to the mass ratio of 7:93, mixing, fully stirring at room temperature until the spinning solution is transparent and uniform, carrying out electrostatic spinning on the formed spinning solution, wherein the voltage is 18kV, the receiving distance is 12cm, the flow rate is 1mL/h, drying a product obtained by spinning, placing the product in a tubular furnace, carrying out heat treatment at 330 ℃ for 2h in air atmosphere, and then carrying out heat treatment at 850 ℃ for 2h in nitrogen atmosphere to obtain carbon nanofibers;
2) Immersing 5g of carbon nanofiber into a silver-ammonia solution consisting of 45mL of ethanol, 0.6g of silver nitrate and 5mL of ammonia water, taking out after immersing for 8 hours, putting into 60mL of polyvinylpyrrolidone ethanol solution with the concentration of 25mg/mL, and reacting for 4 hours at the temperature of 75 ℃ and under the condition of 80r/min to obtain pretreated carbon nanofiber;
3) 3g of the pretreated carbon nanofiber was immersed in 80mL of a 6.7mg/mL silver nitrate and citric acid complex aqueous solution, wherein the molar ratio of silver nitrate to citric acid was 1:1.1, then dropwise adding 26mL of 13mg/mL ascorbic acid aqueous solution, continuously reacting for 7h at 200W and 150r/min, repeatedly washing with ultrapure water after the reaction is finished, and drying to obtain the composite fiber.
A preparation method of a capsule type concentrated detergent specifically comprises the following steps:
1) Weighing the components according to the parts by weight, firstly adding sodium fatty alcohol polyoxyethylene ether sulfate, alkyl glycoside and modified silicone oil into a half amount of water/oil emulsion, stirring for 30min at 700r/min, then dropwise adding a half amount of calcium chloride-containing chitosan solution under stirring, continuing stirring for 40min after the dropwise adding, then demulsifying and layering with isopropanol, and repeatedly washing with distilled water while vacuum filtration to obtain a microcapsule A;
2) Adding enzyme into the rest half of water/oil emulsion, stirring at 700r/min for 30min, then dropwise adding the rest half of chitosan solution containing calcium chloride under stirring, continuing stirring for 40min after dropwise adding, then demulsifying and layering with isopropanol, vacuum filtering, and repeatedly washing with distilled water to obtain microcapsule B;
3) Adding sodium dodecyl sulfonate, citric acid, hydantoin and an auxiliary agent into a gelatin solution, stirring at a temperature of 38 ℃ for 25min at 1300r/min, then adding a microcapsule A and a microcapsule B, stirring at a temperature of 200r/min for 15min to obtain an emulsion, adding a flocculating agent into the emulsion under the stirring of 350r/min, dividing the flocculating agent into 6 equal parts, adding one part every 8min, adding a composite fiber into the emulsion after the mixture is encapsulated, continuing stirring for 35min, and dropwise adding n-butanol as an antifoaming agent for defoaming in the encapsulation process, wherein the whole process keeps stirring and maintains the temperature at 37 ℃, thus obtaining microcapsule particles;
4) And (3) placing the microcapsules in ice water for cooling, stirring at 150r/min until the microcapsules are completely condensed, adding glutaraldehyde for solidification for 3 hours, standing the microcapsule solution, precipitating, pouring out the upper liquid and recovering the flocculant, and freeze-drying the microcapsules at the bottom layer to obtain the required capsule type concentrated detergent.
Example 3
The capsule type concentrated detergent is characterized by comprising the following components in parts by weight: 40 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 20 parts of alkyl glycoside, 15 parts of modified silicone oil, 30 parts of sodium dodecyl sulfate, 3 parts of citric acid, 1 part of enzyme, 0.1 part of hydantoin, 15 parts of auxiliary agent, 120 parts of water/oil emulsion, 80 parts of calcium chloride-containing chitosan solution, 70 parts of gelatin solution, 3 parts of flocculant, 7 parts of composite fiber and 5 parts of glutaraldehyde;
the preparation method of the water/oil type emulsion comprises the following steps:
emulsifying 10mL of sodium alginate solution with the concentration of 6wt% into 50mL of liquid paraffin containing 8wt% span-80, and magnetically stirring for 30 min;
the preparation method of the chitosan solution containing calcium chloride comprises the following steps:
taking 20mL of distilled water, adding acetic acid according to the proportion of 3wt%, uniformly mixing, adding 7g of chitosan, fully stirring and dissolving, adding 1.2g of calcium chloride, and fully stirring;
the preparation method of the modified silicone oil comprises the following steps:
Dissolving 3g of dry chloroplatinic acid in 100mL of distilled isopropanol, fully stirring, standing overnight to obtain a product A, adding 15g allyl polyether and 8g hydrogen-containing silicone oil into a container, introducing enough nitrogen to exhaust air, heating to 80 ℃, dropwise adding 0.5g of the product A, stirring at 100r/min for reaction for 6h, and distilling under reduced pressure to remove low-boiling substances after the reaction is finished to obtain modified silicone oil, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.75%, the viscosity is 54mm 2/s, and the molecular weight of the allyl polyether is 500.
The preparation method of the composite fiber comprises the following steps:
1) Polyacrylonitrile and N, N-dimethylformamide are mixed according to the mass ratio of 8:92, fully stirring at room temperature until the spinning solution is transparent and uniform, carrying out electrostatic spinning on the formed spinning solution, wherein the voltage is 20kV, the receiving distance is 15cm, the flow rate is 1.5mL/h, drying a product obtained by spinning, placing the product in a tubular furnace, carrying out heat treatment for 3h at 350 ℃ in air atmosphere, and then carrying out heat treatment for 3h at 860 ℃ in nitrogen atmosphere to obtain carbon nanofibers;
2) Immersing 8g of carbon nanofiber into a silver-ammonia solution consisting of 50mL of ethanol, 0.9g of silver nitrate and 6mL of ammonia water, taking out after immersing for 10 hours, putting into 70mL of polyvinylpyrrolidone ethanol solution with the concentration of 30mg/mL, and reacting for 5 hours at the temperature of 76 ℃ and under the condition of 100r/min to obtain pretreated carbon nanofiber;
3) 5g of the pretreated carbon nanofiber is immersed in 100mL of a 7mg/mL silver nitrate and citric acid composite aqueous solution, wherein the molar ratio of the silver nitrate to the citric acid is 1:1.2, then 28mL of 15mg/mL ascorbic acid aqueous solution is dropwise added, the reaction is continued for 9 hours under 200W and 180r/min, after the reaction is finished, the composite fiber is obtained after repeated washing with ultrapure water and drying.
A preparation method of a capsule type concentrated detergent specifically comprises the following steps:
1) Weighing the components according to the parts by weight, firstly adding sodium fatty alcohol polyoxyethylene ether sulfate, alkyl glycoside and modified silicone oil into a half amount of water/oil emulsion, stirring for 40min at 800r/min, then dropwise adding a half amount of calcium chloride-containing chitosan solution under stirring, continuing stirring for 50min after the dropwise adding, then demulsifying and layering with isopropanol, and repeatedly washing with distilled water while vacuum filtration to obtain a microcapsule A;
2) Adding enzyme into the rest half of water/oil emulsion, stirring for 40min at 800r/min, then dropwise adding the rest half of chitosan solution containing calcium chloride under stirring, continuing stirring for 50min after dropwise adding, then demulsifying and layering with isopropanol, vacuum filtering, and repeatedly washing with distilled water to obtain microcapsule B;
3) Adding sodium dodecyl sulfonate, citric acid, hydantoin and an auxiliary agent into a gelatin solution, stirring at 40 ℃ for 30min at 1500r/min, then adding a microcapsule A and a microcapsule B, stirring at 300r/min for 20min to obtain an emulsion, adding a flocculating agent into the emulsion under 400r/min stirring, dividing the flocculating agent into 8 equal parts, adding one part every 10min, adding a composite fiber into the emulsion after the mixture is encapsulated, continuing stirring for 40min, and dropwise adding n-butanol as an antifoaming agent for defoaming in the encapsulation process, wherein the whole process keeps stirring and maintains the temperature at 40 ℃, thus obtaining microcapsule particles;
4) And (3) placing the microcapsules in ice water for cooling, stirring at 180r/min until the microcapsules are completely condensed, adding glutaraldehyde for solidification for 4 hours, standing the microcapsule solution, precipitating, pouring out the upper liquid and recovering the flocculant, and freeze-drying the microcapsules at the bottom layer to obtain the required capsule type concentrated detergent.
Comparative example 1: this comparative example is substantially the same as example 1 except that no modified silicone oil is contained.
Comparative example 2: this comparative example is substantially the same as example 1 except that the active agent component is not subjected to the microencapsulation treatment.
Comparative example 3: this comparative example is substantially the same as example 1 except that the enzyme was not subjected to the microencapsulation treatment.
Comparative example 4: this comparative example is substantially the same as example 1 except that no conjugate fiber is added during the preparation of the capsule type concentrated detergent.
Comparative example 5: this comparative example is substantially the same as example 1 except that carbon nanofibers are used instead of the composite fibers in the preparation of the capsule type concentrated detergent.
Test experiment:
The procedure of examples 1 to 3 and comparative examples 1 to 5 was used to prepare a concentrated detergent sample in the form of a capsule, and the detergency was measured by the foam level method of method 2 for measuring detergency of annex B of GB 9985-2000 national Standard hand dishwashing detergent for people's republic of China, and the results were as follows:
| example 1 | Example 2 | Example 3 | Comparative example 1 | |
| Detergency (personal) | 5.3 | 5.8 | 5.6 | 2.3 |
| Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | |
| Detergency (personal) | 2.6 | 2.5 | 3.7 | 4.2 |
As shown in the table, the capsule type concentrated detergent has excellent detergency, can remove greasy dirt rapidly, and achieves the effect of cleaning tableware efficiently.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (5)
1. The preparation method of the capsule type concentrated detergent is characterized by comprising the following steps of:
1) Weighing the components according to the parts by weight, adding sodium fatty alcohol polyoxyethylene ether sulfate, alkyl glycoside and modified silicone oil into a half amount of water/oil type emulsion, fully stirring, dropwise adding a half amount of calcium chloride-containing chitosan solution under stirring, continuing stirring after the dropwise adding, then demulsifying and layering by isopropanol, vacuum filtering, and repeatedly washing by distilled water to obtain a microcapsule A;
2) Adding enzyme into a half amount of water/oil emulsion, fully stirring, then dropwise adding a half amount of chitosan solution containing calcium chloride under stirring, continuing stirring after the dropwise adding, then demulsifying and layering by isopropanol, and repeatedly washing by distilled water while vacuum filtration to obtain a microcapsule B;
3) Adding sodium dodecyl sulfonate, citric acid, hydantoin and an auxiliary agent into a gelatin solution, fully stirring at 35-40 ℃, adding a microcapsule A and a microcapsule B to obtain emulsion, adding a flocculating agent into the emulsion under stirring, dividing the flocculating agent into 5-8 equal parts, adding one part every 5-10min, adding a composite fiber into the mixture after encapsulation, and keeping stirring and maintaining the temperature at 35-40 ℃ in the whole process to obtain microcapsule particles;
4) Placing microcapsule particles in ice water for cooling, stirring until the microcapsule particles are completely condensed, adding glutaraldehyde for solidification for 2-4 hours, standing microcapsule solution, precipitating, pouring out upper liquid and recovering flocculant, and freeze-drying the microcapsules at the bottom layer to obtain the required capsule type concentrated detergent;
the weight portions of the components are as follows: 25-40 parts of fatty alcohol polyoxyethylene ether sodium sulfate, 10-20 parts of alkyl glycoside, 8-15 parts of modified silicone oil, 15-30 parts of sodium dodecyl sulfate, 0.5-3 parts of citric acid, 0.3-1 part of enzyme, 0.05-0.1 part of hydantoin, 6-15 parts of auxiliary agent, 80-120 parts of water/oil emulsion, 50-80 parts of calcium chloride-containing chitosan solution, 50-70 parts of gelatin solution, 1-3 parts of flocculant, 3-7 parts of composite fiber and 2-5 parts of glutaraldehyde;
the preparation method of the water/oil type emulsion comprises the following steps: emulsifying 5-10mL of sodium alginate solution with concentration of 2-6wt% into 30-50mL of liquid paraffin containing 5-8wt% span-80, and magnetically stirring for 10-30 min;
the preparation method of the chitosan solution containing calcium chloride comprises the following steps: adding acetic acid into 10-20mL of distilled water according to the proportion of 1-3wt%, uniformly mixing, adding 3-7g of chitosan, fully stirring and dissolving, adding 0.6-1.2g of calcium chloride, and fully stirring;
the preparation method of the composite fiber comprises the following steps:
1) Carrying out electrostatic spinning on spinning solution formed by mixing polyacrylonitrile and N, N-dimethylformamide, drying a spinning product, placing the spinning product in a tubular furnace, carrying out heat treatment for 1-3h at 300-350 ℃ in air atmosphere, and then carrying out heat treatment for 1-3h at 800-860 ℃ in nitrogen atmosphere to obtain carbon nanofibers;
2) Immersing the carbon nanofiber into a silver-ammonia solution composed of ethanol, silver nitrate and ammonia water, immersing for 5-10h, taking out, putting into a polyvinylpyrrolidone ethanol solution, and stirring and reacting for 3-5h at 70-76 ℃ to obtain the pretreated carbon nanofiber;
3) Immersing the pretreated carbon nanofiber into a silver nitrate and citric acid composite aqueous solution, dropwise adding an ascorbic acid aqueous solution, continuously reacting for 4-9 hours under ultrasonic and stirring, repeatedly washing with ultrapure water after the reaction is finished, and drying to obtain the composite fiber;
Wherein the mass ratio of the polyacrylonitrile to the N, N-dimethylformamide is (5-8): (92-95);
The electrostatic spinning voltage is 15-20kV, the receiving distance is 10-15cm, and the flow rate is 0.5-1.5mL/h;
The dosage proportion of the carbon nanofiber, ethanol, silver nitrate, ammonia water and polyvinylpyrrolidone ethanol solution is (3-8) g: (40-50) mL: (0.4-0.9) g: (3-6) mL: (50-70) mL;
The concentration of the polyvinylpyrrolidone ethanol solution is 20-30mg/mL;
The dosage proportion of the pretreated carbon nanofiber, the silver nitrate and citric acid composite aqueous solution and the ascorbic acid aqueous solution is (2-5) g: (70-100) mL: (20-28) mL;
The concentration of the silver nitrate and citric acid composite aqueous solution is 6.5-7.0mg/mL, wherein the molar ratio of the silver nitrate to the citric acid is 1: (1.0-1.2);
The concentration of the ascorbic acid aqueous solution is 10-15mg/mL.
2. The preparation method of the capsule type concentrated detergent as claimed in claim 1, wherein the enzyme comprises proteinase K and papain according to a mass ratio of 1: (1-3);
The auxiliary agent is prepared from urea, ethylenediamine tetraacetic acid, salt, sodium benzoate and trisodium citrate according to the mass ratio of 1: (0.2-0.6): (0.6-1.3): (1-3): (0.1-0.7);
The concentration of the gelatin solution is 5-8wt%;
The flocculant is prepared from sodium sulfate and ammonium sulfate according to a mass ratio of 1: (1.0-1.5).
3. The method for preparing the capsule-type concentrated detergent as claimed in claim 1, wherein the preparation method of the modified silicone oil is as follows: dissolving dry chloroplatinic acid in distilled isopropanol, fully stirring, standing overnight to obtain a product A, adding allyl polyether and hydrogen-containing silicone oil into a container, introducing enough nitrogen to exhaust air, heating to 60-80 ℃, then dropwise adding the product A, stirring for reacting for 4-6h, and after the reaction is finished, distilling under reduced pressure to remove low-boiling substances to obtain the modified silicone oil.
4. A method for preparing a concentrated detergent in capsule form according to claim 3, wherein the ratio of chloroplatinic acid to isopropyl alcohol is (1-3) g: (60-100) mL;
The mass ratio of the allyl polyether to the hydrogen-containing silicone oil to the product A is (10-15): (5-8): (0.1-0.5).
5. The method for preparing a concentrated detergent in capsule form according to claim 4, wherein the hydrogen content of the hydrogen-containing silicone oil is 0.18-0.75%, and the viscosity is 54-152mm 2/s;
The molecular weight of the allyl polyether is 300-600.
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| CN102453627A (en) * | 2010-10-25 | 2012-05-16 | 郑建明 | Cleaning agent for residual pesticides on fruit and vegetable |
| EP3137587B1 (en) * | 2014-05-02 | 2018-09-12 | Novozymes A/S | Detergent composition |
| CN104017668A (en) * | 2014-06-05 | 2014-09-03 | 广州立白企业集团有限公司 | Emulsus dish washing detergent |
| CN105037768A (en) * | 2015-08-30 | 2015-11-11 | 常州亚环环保科技有限公司 | Method for preparing organic silicon modified chitosan membrane |
| CN105542972A (en) * | 2015-12-16 | 2016-05-04 | 天津兰黛采妆环保科技开发有限公司 | Environmentally friendly tableware-dedicated cleaning paste |
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