CN111423940B - 一种含有山茶油洗涤剂的制备工艺 - Google Patents
一种含有山茶油洗涤剂的制备工艺 Download PDFInfo
- Publication number
- CN111423940B CN111423940B CN202010293468.XA CN202010293468A CN111423940B CN 111423940 B CN111423940 B CN 111423940B CN 202010293468 A CN202010293468 A CN 202010293468A CN 111423940 B CN111423940 B CN 111423940B
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- Prior art keywords
- camellia oil
- reaction
- antibacterial
- sodium
- product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000010495 camellia oil Substances 0.000 title claims abstract description 66
- 239000003599 detergent Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 77
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 70
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003607 modifier Substances 0.000 claims abstract description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 17
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229940080421 coco glucoside Drugs 0.000 claims abstract description 9
- 235000019864 coconut oil Nutrition 0.000 claims abstract description 9
- 239000003240 coconut oil Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 9
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000194 fatty acid Substances 0.000 claims abstract description 9
- 229930195729 fatty acid Natural products 0.000 claims abstract description 9
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 9
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 9
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 9
- 239000011780 sodium chloride Substances 0.000 claims abstract description 9
- 239000001509 sodium citrate Substances 0.000 claims abstract description 9
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 9
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 9
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims abstract description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 8
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims abstract description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 25
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 21
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 20
- 238000004821 distillation Methods 0.000 claims description 17
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000003921 oil Substances 0.000 claims description 9
- 235000019198 oils Nutrition 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 6
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 6
- 239000001632 sodium acetate Substances 0.000 claims description 6
- 235000017281 sodium acetate Nutrition 0.000 claims description 6
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 5
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims description 5
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000011541 reaction mixture Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- KJRFTNVYOAGTHK-UHFFFAOYSA-N methyl 3-hydroxy-2,2-dimethylpropanoate Chemical compound COC(=O)C(C)(C)CO KJRFTNVYOAGTHK-UHFFFAOYSA-N 0.000 claims 1
- LDTLDBDUBGAEDT-UHFFFAOYSA-N methyl 3-sulfanylpropanoate Chemical compound COC(=O)CCS LDTLDBDUBGAEDT-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- MGIYRDNGCNKGJU-UHFFFAOYSA-N isothiazolinone Chemical compound O=C1C=CSN1 MGIYRDNGCNKGJU-UHFFFAOYSA-N 0.000 description 20
- 150000003242 quaternary ammonium salts Chemical group 0.000 description 16
- 230000007794 irritation Effects 0.000 description 14
- VUWCWMOCWKCZTA-UHFFFAOYSA-N 1,2-thiazol-4-one Chemical group O=C1CSN=C1 VUWCWMOCWKCZTA-UHFFFAOYSA-N 0.000 description 11
- 229940017219 methyl propionate Drugs 0.000 description 6
- 241000588724 Escherichia coli Species 0.000 description 4
- 241000191967 Staphylococcus aureus Species 0.000 description 4
- 230000003110 anti-inflammatory effect Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 230000001050 lubricating effect Effects 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 230000000638 stimulation Effects 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 239000002085 irritant Substances 0.000 description 2
- 231100000021 irritant Toxicity 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229940100555 2-methyl-4-isothiazolin-3-one Drugs 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- BEGLCMHJXHIJLR-UHFFFAOYSA-N methylisothiazolinone Chemical compound CN1SC=CC1=O BEGLCMHJXHIJLR-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- TZYULTYGSBAILI-UHFFFAOYSA-M trimethyl(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC=C TZYULTYGSBAILI-UHFFFAOYSA-M 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/83—Mixtures of non-ionic with anionic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/02—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols
- C07C319/12—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols by reactions not involving the formation of mercapto groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D275/00—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings
- C07D275/02—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings not condensed with other rings
- C07D275/03—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
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- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B5/00—Preserving by using additives, e.g. anti-oxidants
- C11B5/0071—Preserving by using additives, e.g. anti-oxidants containing halogens, sulfur or phosphorus
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/044—Hydroxides or bases
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2086—Hydroxy carboxylic acids-salts thereof
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/33—Amino carboxylic acids
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/382—Vegetable products, e.g. soya meal, wood flour, sawdust
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/50—Perfumes
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/29—Sulfates of polyoxyalkylene ethers
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/662—Carbohydrates or derivatives
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- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Detergent Compositions (AREA)
Abstract
本发明公开了一种含有山茶油洗涤剂的制备工艺,具体制备过程如下:将去离子水入反应釜中,然后向其中加入椰油基葡糖苷、脂肪醇聚氧乙烯醚硫酸钠、十二烷基苯磺酸钠、椰子油脂肪酸二乙醇酰胺、氯化钠、氢氧化钠、柠檬酸钠和乙二胺四乙酸二钠,搅拌混合均匀后向其中加入第一步中制备的抗菌山茶油和香精,搅拌混合均匀后得到洗涤剂。本发明通过在抗菌改性剂中引入硅氧烷键,提高了抗菌改性剂的温度范围,进而使得制备的抗菌改性剂在较高温度下仍具有较高的抗菌性能,在其对山茶油进行改进后,制备的抗菌山茶油同样也具有一定的耐高温性能。
Description
技术领域
本发明属于洗涤剂制备领域,涉及一种含有山茶油洗涤剂的制备工艺。
背景技术
餐具洗涤过程中不仅需要将污垢清洗干净,同时需要对餐具进行杀菌消毒,异噻唑啉酮具有抗菌能力强、应用剂量小、相容性好、并且对多种细菌、真菌都具有很强的抗菌作用,具有它们高效性、较好的配伍性、较宽的pH适用范围,并且能够自然生物降解,被广泛应用于洗涤剂中,但是异噻唑啉酮有腐蚀性在使用洗涤剂进行大量餐具的清洗时,会对手部造成一定的刺激,不适。同时由于异噻唑啉酮的耐高温性能较差,在高温下放置一段时间后会影响其抗菌性能。
发明内容
本发明的目的在于提供一种含有山茶油洗涤剂的制备工艺,通过在洗涤剂中添加抗菌山茶油,实现高效的抗菌性能,同时由于抗菌山茶油中含有异噻唑啉酮基团以及季铵盐基团,两者结合作用能够实现高效的抗菌性能,同时由于异噻唑啉酮具有一定的刺激性能,虽然在清洗剂中加入量较少但是仍对皮肤有一定的刺激性,通过引入季铵盐基团,进而减少了异噻唑啉酮加入量,并且由于山茶油本身也具有一定的抗菌消炎效果,进而使得异噻唑啉酮的加入量较少,减少了刺激,同时山茶油具有一定的护肤润滑作用,能够有效的实现对皮肤的防护作用,防止在使用清洗剂进行清洗时对皮肤的刺激。
本发明的目的可以通过以下技术方案实现:
一种含有山茶油的洗涤剂,包括如下质量分数的各组分:
椰油基葡糖苷1.1-1.2%、脂肪醇聚氧乙烯醚硫酸钠12.3-12.8%、十二烷基苯磺酸钠7.6-8.2%、椰子油脂肪酸二乙醇酰胺1.9-2.1%、氯化钠2.1-2.2%、氢氧化钠1.3-1.5%、柠檬酸钠0.4-0.5%、抗菌山茶油2.2-2.3%、乙二胺四乙酸二钠0.2-0.3%、香精0.08-0.09%、去离子水余量;
抗菌山茶油的具体制备过程如下:
步骤1:将甲醇钠和乙醚同时加入反应容器中,升温至55-60℃,然后向其中加入2,2-二甲基-3-羟基丙酸甲酯,搅拌混合均匀后向其中逐滴加入3-巯基丙酸甲酯,滴加完全后恒温搅拌反应3-4h,然后向其中加入三氯乙烯和水进行稀释,接着用稀盐酸调节溶液的pH=1,并将溶液倒入分液漏斗中进行静止分液,取上层油相用无水硫酸钠干燥,然后进行减压蒸馏,得到产物A,反应结构式如下所示;其中2,2-二甲基-3-羟基丙酸甲酯和3-巯基丙酸甲酯按照质量比为1:1的比例加入;2,2-二甲基-3-羟基丙酸甲酯和3-巯基丙酸甲酯两种酯在碱性条件下发生酯缩合反应,2,2-二甲基-3-羟基丙酸甲酯中羰基邻位碳上没有氢原子,而3-巯基丙酸甲酯中羰基邻位上的氢原子具有一定的活性,能够进行缩合反应;
步骤2:将产物A加入反应容器中,然后向其中加入浓氨水,常温下反应8-9h,然后进行减压蒸馏,得到产物B;反应结构式如下所示,其中每克产物A中加入浓氨水8.5-9mL;
步骤3:将产物B、磺酰氯和二氯甲烷同时加入反应釜中,升温至70-75℃回流反应3-4h,然后进行抽滤,将得到的固体粉末加入水中溶解后再向其中加入氨水调节溶液的pH=8-8.5,然后进行减压蒸馏,并将得到的产物用乙酸乙酯进行重结晶,得到产物C,反应结构式如下所示;其中产物B与磺酰氯按照物质的量之比为1:1.98-2.01的比例加入;
步骤4:称取一定量的甲基丙烯酸二甲氨基乙酯、3-氯丙基三乙氧基硅烷和无水乙醇加入反应容器中,升温至75-80℃回流反应4-5h,然后蒸发除去其中的溶剂后降温至5-10℃,再向反应容器中加入二氯甲烷和乙酸钠,搅拌混合均匀后向反应容器中逐滴加入质量浓度为50%的过氧乙酸溶液,滴加完全后恒温反应6-7h,然后再向其中加入碳酸钠溶液,调节pH=9,并将产物溶液加入分液漏斗中进行静置分液,然后将油相进行减压蒸馏,得到产物D,反应结构式如下所示;其中每克甲基丙烯酸二甲氨基乙酯中加入1.58-1.61g3-氯丙基三乙氧基硅烷,加入乙酸钠0.21-0.22g,加入质量浓度为50%的过氧乙酸溶液3.2-3.4g;
步骤5:将产物C、产物D和丙酮同时加入反应容器中,然后升温至70-80℃,搅拌回流6-7h,然后将得到的产物进行减压蒸馏,得到抗菌改性剂,反应结构式如下所示,其中每克产物C中加入1.9-2.1g产物D;由于产物D中含有环氧基团,同时产物C中的氨基上含有活泼氢,能够与环氧基团进行开环反应,进而在制备的产物中引入羟基;
步骤6:称取一定量的山茶油加入反应釜中,然后向其中加入步骤5中制备的抗菌改性剂,升温至150℃后向其中加入对甲苯磺酸,控制反应釜的压强在0.09MPa,持续加热反应9-10h,然后用80℃的热水将反应混合物反复洗涤4次,分去水层后除去对甲苯磺酸,然后用无水氯化钙进行干燥后得到抗菌山茶油;其中每100克山茶油中加入抗菌改性剂6.8-7.1g,对甲苯磺酸的加入量为山茶油和抗菌改性剂总加入量的1.2-1.3%,由于抗菌改性剂中含有异噻唑啉酮基团以及季铵盐基团,两者结合作用能够实现高效的抗菌性能,同时由于异噻唑啉酮具有一定的刺激性能,虽然在清洗剂中加入量较少但是仍对皮肤有一定的刺激性,通过引入季铵盐基团,进而减少了异噻唑啉酮加入量,并且由于山茶油本身也具有一定的抗菌消炎效果,进而使得异噻唑啉酮的加入量较少,减少了刺激,同时山茶油具有一定的护肤润滑作用,能够有效的实现对皮肤的防护作用,防止在使用清洗剂进行清洗时对皮肤的刺激;
一种含有山茶油洗涤剂的制备工艺,具体制备过程如下:
将去离子水入反应釜中,然后向其中加入椰油基葡糖苷、脂肪醇聚氧乙烯醚硫酸钠、十二烷基苯磺酸钠、椰子油脂肪酸二乙醇酰胺、氯化钠、氢氧化钠、柠檬酸钠和乙二胺四乙酸二钠,搅拌混合均匀后向其中加入抗菌山茶油和香精,搅拌混合均匀后得到洗涤剂。
本发明的有益效果:
1、本发明通过在洗涤剂中添加抗菌山茶油,实现高效的抗菌性能,同时由于抗菌山茶油中含有异噻唑啉酮基团以及季铵盐基团,两者结合作用能够实现高效的抗菌性能,同时由于异噻唑啉酮具有一定的刺激性能,虽然在清洗剂中加入量较少但是仍对皮肤有一定的刺激性,通过引入季铵盐基团,进而减少了异噻唑啉酮加入量,并且由于山茶油本身也具有一定的抗菌消炎效果,进而使得异噻唑啉酮的加入量较少,减少了刺激,同时山茶油具有一定的护肤润滑保湿作用,能够有效的实现对皮肤的防护作用,防止在使用清洗剂进行清洗时对皮肤的刺激。
2、本发明通过在抗菌改性剂中引入硅氧烷键,提高了抗菌改性剂的温度范围,进而使得制备的抗菌改性剂在较高温度下仍具有较高的抗菌性能,在其对山茶油进行改进后,制备的抗菌山茶油同样也具有一定的耐高温性能。
3、本发明制备的抗菌改性剂中直接引入有氧基硅烷键、异噻唑啉酮基团和季铵盐基团,使得三种功能基团的含量稳定,进而使得在制备洗涤剂过程中,三种基团的含量比例稳定,并且作用位点位置固定,进而有效直接添加含有三种功能基团的助剂时,造成其分部不均匀,进而影响作用效果。
具体实施方式
实施例1:
抗菌山茶油的具体制备过程如下:
步骤1:将4.3g甲醇钠和乙醚同时加入反应容器中,升温至55-60℃,然后向其中加入10g2,2-二甲基-3-羟基丙酸甲酯,搅拌混合均匀后向其中逐滴加入10g3-巯基丙酸甲酯,滴加完全后恒温搅拌反应3-4h,然后向其中加入三氯乙烯和水进行稀释,接着用稀盐酸调节溶液的pH=1,并将溶液倒入分液漏斗中进行静止分液,取上层油相用无水硫酸钠干燥,然后进行减压蒸馏,得到产物A,反应结构式如下所示;
步骤2:将10g产物A加入反应容器中,然后向其中加入85mL浓氨水,常温下反应8-9h,然后进行减压蒸馏,得到产物B,反应结构式如下所示;
步骤3:将10.2g产物B、6.7g磺酰氯和120mL二氯甲烷同时加入反应釜中,升温至70-75℃回流反应3-4h,然后进行抽滤,将得到的固体粉末加入水中溶解后再向其中加入氨水调节溶液的pH=8-8.5,然后进行减压蒸馏,并将得到的产物用乙酸乙酯进行重结晶,得到产物C,反应结构式如下所示;
步骤4:称取10g甲基丙烯酸二甲氨基乙酯、15.8g3-氯丙基三乙氧基硅烷和160mL无水乙醇加入反应容器中,升温至75-80℃回流反应4-5h,然后蒸发除去其中的溶剂后降温至5-10℃,再向反应容器中加入120mL二氯甲烷和2.1g乙酸钠,搅拌混合均匀后向反应容器中逐滴加入32g质量浓度为50%的过氧乙酸溶液,滴加完全后恒温反应6-7h,然后再向其中加入碳酸钠溶液,调节pH=9,并将产物溶液加入分液漏斗中进行静置分液,然后将油相进行减压蒸馏,得到产物D,反应结构式如下所示;
步骤5:将10g产物C、19g产物D和250mL丙酮同时加入反应容器中,然后升温至70-80℃,搅拌回流6-7h,然后将得到的产物进行减压蒸馏,得到抗菌改性剂,反应结构式如下所示;
步骤6:称取20g山茶油加入反应釜中,然后向其中加入1.4g步骤5中制备的抗菌改性剂,升温至150℃后向其中加入0.25g对甲苯磺酸,控制反应釜的压强在0.09MPa,持续加热反应9-10h,然后用80℃的热水将反应混合物反复洗涤4次,分去水层后除去对甲苯磺酸,然后用无水氯化钙进行干燥后得到抗菌山茶油。
实施例2:
抗菌山茶油的具体制备过程如下:
步骤1:称取10g烯丙基三甲基氯化铵加入80mL二氯甲烷和2.1g乙酸钠,搅拌混合均匀后向反应容器中逐滴加入32g质量浓度为50%的过氧乙酸溶液,滴加完全后恒温反应6-7h,然后再向其中加入碳酸钠溶液,调节pH=9,并将产物溶液加入分液漏斗中进行静置分液,然后将油相进行减压蒸馏,得到产物D,
步骤2:将10g实施例1中制备的产物C、步骤1中制备的19g产物D和250mL丙酮同时加入反应容器中,然后升温至70-80℃,搅拌回流6-7h,然后将得到的产物进行减压蒸馏,得到抗菌改性剂;
步骤3:称取20g山茶油加入反应釜中,然后向其中加入1.4g步骤5中制备的抗菌改性剂,升温至150℃后向其中加入0.25g对甲苯磺酸,控制反应釜的压强在0.09MPa,持续加热反应9-10h,然后用80℃的热水将反应混合物反复洗涤4次,分去水层后除去对甲苯磺酸,然后用无水氯化钙进行干燥后得到抗菌山茶油。
实施例3:
一种含有山茶油洗涤剂的制备工艺,具体制备过程如下:
将去离子水入反应釜中,然后向其中加入椰油基葡糖苷、脂肪醇聚氧乙烯醚硫酸钠、十二烷基苯磺酸钠、椰子油脂肪酸二乙醇酰胺、氯化钠、氢氧化钠、柠檬酸钠和乙二胺四乙酸二钠,搅拌混合均匀后向其中加入实施例1中制备的抗菌山茶油和香精,搅拌混合均匀后得到洗涤剂;其中各组分的含量如下:椰油基葡糖苷1.2%、脂肪醇聚氧乙烯醚硫酸钠12.8%、十二烷基苯磺酸钠8.2%、椰子油脂肪酸二乙醇酰胺2.1%、氯化钠2.2%、氢氧化钠1.5%、柠檬酸钠0.5%、抗菌山茶油2.3%、乙二胺四乙酸二钠0.3%、香精0.09%、去离子水余量;
实施例4:
一种含有山茶油洗涤剂的制备工艺,具体制备过程如下:
将去离子水入反应釜中,然后向其中加入椰油基葡糖苷、脂肪醇聚氧乙烯醚硫酸钠、十二烷基苯磺酸钠、椰子油脂肪酸二乙醇酰胺、氯化钠、氢氧化钠、柠檬酸钠和乙二胺四乙酸二钠,搅拌混合均匀后向其中加入实施例2中制备的抗菌山茶油和香精,搅拌混合均匀后得到洗涤剂;其中各组分的含量如下:椰油基葡糖苷1.1%、脂肪醇聚氧乙烯醚硫酸钠12.3%、十二烷基苯磺酸钠7.6%、椰子油脂肪酸二乙醇酰胺1.9%、氯化钠2.1%、氢氧化钠1.3%、柠檬酸钠0.4%、实施例2中制备的抗菌山茶油2.2%、乙二胺四乙酸二钠0.2%、香精0.08%、余量去离子水。
实施例5:
一种洗涤剂的制备工艺,具体制备过程与实施例3相同,将实施例3中使用的实施例2中制备的抗菌山茶油替换为实施例1制备的抗菌改性剂。
实施例6:
一种洗涤剂的制备工艺,具体制备过程与实施例3相同,将实施例3中使用的实施例2中制备的抗菌山茶油替换为2-甲基-4-异噻唑啉-3-酮。
实施例7:
一种含有山茶油洗涤剂的制备工艺,具体制备过程与实施例3相同,将实施例3中使用的实施例2中制备的抗菌山茶油替换为山茶油。
实施例8:
将实施例3-7中制备的洗涤剂分别在温度为20℃、30℃和50℃下放置3天,将大肠杆菌和金黄色葡萄球菌分别接种于合适的培养基中,于25℃下培养3天后,挑选典型的菌落于灭菌的液体培养基中制成一定浓度的悬液,其中控制大肠杆菌和金黄色葡萄球菌每克悬液含菌量为1X 106CFU/g或CFU/ml,然后根据QB/T2738-2005标准,采用悬浮定量法测定实施例3-7中的洗涤剂在不同温度下放置一段时间后对大肠杆菌和金黄色葡萄球菌的抑菌率,稀释后的洗涤剂与悬液混合时温度为30℃,具体测定结果如表1所示:
表1:大肠杆菌和金黄色葡萄球菌的抑菌率测试结果
由表1可知,实施例3、实施例5中制备的洗涤剂具有一定的耐热性能,在较高温度下放置一段时间后其抗菌性能仍没有任何变化,因为制备的抗菌山茶油中引入有硅氧烷键,进而提高了洗涤剂中抗菌山茶油的耐温范围,而实施例4和实施例6中洗涤剂在高温下放置一段时间后期抗菌性能稍有降低,由于添加的抗菌成分中含有异噻唑啉酮基团,其储存温度只有-10-40℃,耐高温性能较差,使用温度范围较低,进而影响洗涤剂的存储和使用,并且异噻唑啉酮基团和季铵盐基团两者结合作用能够实现高效的抗菌性能,同时山茶油本身具有一定的抗菌性能,进而使得制备的洗涤剂在添加抗菌剂含量一定时,减少异噻唑啉酮的含量时其抗菌性能仍没有变化,进而能够有效较少洗涤剂的刺激作用。
实施例9:
选取50个志愿者,10个为一组,不同组使用实施例3-7中的洗涤剂对盘子进行重油的盘子进行清洗,每人清洗20个盘子,然后记录每组志愿者手部的不同感受,结果如表2所示;
表2实施例3-7中制备的洗涤剂使用过程中对皮肤的刺激结果
由表2可知,实施例3、实施例4和实施例7中制备的洗涤剂性能温和无刺激,使用过程中不会对皮肤造成损伤,由于其中含有山茶油成分,并且由于异噻唑啉酮具有一定的刺激性能,虽然在清洗剂中加入量较少但是仍对皮肤有一定的刺激性,通过引入季铵盐基团,进而减少了异噻唑啉酮加入量,并且由于山茶油本身也具有一定的抗菌消炎效果,进而使得异噻唑啉酮的加入量较少,减少了刺激,同时山茶油具有一定的护肤润滑作用,能够有效的实现对皮肤的防护作用,防止在使用清洗剂进行清洗时对皮肤的刺激,而实施例5和6中直接添加抗菌成分,其中含有大量的异噻唑啉酮,进而使得大量清洗过程中对皮肤造成较大刺激。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节,也不限制该发明仅为所述的具体实施方式。显然,根据本说明书的内容,可作很多的修改和变化。本说明书选取并具体描述这些实施例,是为了更好地解释本发明的原理和实际应用,从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。
Claims (6)
1.一种含有山茶油洗涤剂的制备工艺,其特征在于,具体制备过程如下:
第一步:称取一定量的山茶油加入反应釜中,然后向其中加入抗菌改性剂,升温至150℃后向其中加入对甲苯磺酸,控制反应釜的压强在0.09MPa,持续加热反应9-10h,然后用80℃的热水将反应混合物反复洗涤4次,分去水层后除去对甲苯磺酸,然后用无水氯化钙进行干燥后得到抗菌山茶油;
其中抗菌改性剂的具体制备过程如下:
步骤1:将甲醇钠和乙醚同时加入反应容器中,升温至55-60℃,然后向其中加入2,2-二甲基-3-羟基丙酸甲酯,搅拌混合均匀后向其中逐滴加入3-巯基丙酸甲酯,滴加完全后恒温搅拌反应3-4h,然后向其中加入三氯乙烯和水进行稀释,接着用稀盐酸调节溶液的pH=1,并将溶液倒入分液漏斗中进行静止分液,取上层油相用无水硫酸钠干燥,然后进行减压蒸馏,得到产物A,反应结构式如下所示;
步骤2:将产物A加入反应容器中,然后向其中加入浓氨水,常温下反应8-9h,然后进行减压蒸馏,得到产物B,反应结构式如下所示;
步骤3:将产物B、磺酰氯和二氯甲烷同时加入反应釜中,升温至70-75℃回流反应3-4h,然后进行抽滤,将得到的固体粉末加入水中溶解后再向其中加入氨水调节溶液的pH=8-8.5,然后进行减压蒸馏,并将得到的产物用乙酸乙酯进行重结晶,得到产物C,反应结构式如下所示;
步骤4:称取一定量的甲基丙烯酸二甲氨基乙酯、3-氯丙基三乙氧基硅烷和无水乙醇加入反应容器中,升温至75-80℃回流反应4-5h,然后蒸发除去其中的溶剂后降温至5-10℃,再向反应容器中加入二氯甲烷和乙酸钠,搅拌混合均匀后向反应容器中逐滴加入质量浓度为50%的过氧乙酸溶液,滴加完全后恒温反应6-7h,然后再向其中加入碳酸钠溶液,调节pH=9,并将产物溶液加入分液漏斗中进行静置分液,然后将油相进行减压蒸馏,得到产物D,反应结构式如下所示;
步骤5:将产物C、产物D和丙酮同时加入反应容器中,然后升温至70-80℃,搅拌回流6-7h,然后将得到的产物进行减压蒸馏,得到抗菌改性剂,反应结构式如下所示;
第二步,将去离子水入反应釜中,然后向其中加入椰油基葡糖苷、脂肪醇聚氧乙烯醚硫酸钠、十二烷基苯磺酸钠、椰子油脂肪酸二乙醇酰胺、氯化钠、氢氧化钠、柠檬酸钠和乙二胺四乙酸二钠,搅拌混合均匀后向其中加入第一步中制备的抗菌山茶油和香精,其中各原料的质量百分含量如下:椰油基葡糖苷1.1-1.2%、脂肪醇聚氧乙烯醚硫酸钠12.3-12.8%、十二烷基苯磺酸钠7.6-8.2%、椰子油脂肪酸二乙醇酰胺1.9-2.1%、氯化钠2.1-2.2%、氢氧化钠1.3-1.5%、柠檬酸钠0.4-0.5%、抗菌山茶油2.2-2.3%、乙二胺四乙酸二钠0.2-0.3%、香精0.08-0.09%、去离子水余量,搅拌混合均匀后得到洗涤剂。
2.根据权利要求1所述的一种含有山茶油洗涤剂的制备工艺,其特征在于,第一步中每100克山茶油中加入抗菌改性剂6.8-7.1g,对甲苯磺酸的加入量为山茶油和抗菌改性剂总加入量的1.2-1.3%。
3.根据权利要求1所述的一种含有山茶油洗涤剂的制备工艺,其特征在于,步骤1中2,2-二甲基-3-羟基丙酸甲酯和3-巯基丙酸甲酯按照质量比为1:1的比例入。
4.根据权利要求1所述的一种含有山茶油洗涤剂的制备工艺,其特征在于,步骤2中每克产物A中加入浓氨水8.5-9mL。
5.根据权利要求1所述的一种含有山茶油洗涤剂的制备工艺,其特征在于,步骤3中产物B与磺酰氯按照物质的量之比为1:1.98-2.01的比例加入。
6.根据权利要求1所述的一种含有山茶油洗涤剂的制备工艺,其特征在于,每克甲基丙烯酸二甲氨基乙酯中加入1.58-1.61g3-氯丙基三乙氧基硅烷,加入乙酸钠0.21-0.22g,加入质量浓度为50%的过氧乙酸溶液3.2-3.4g。
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