US2982736A - Method of preparedg washing - Google Patents
Method of preparedg washing Download PDFInfo
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- US2982736A US2982736A US2982736DA US2982736A US 2982736 A US2982736 A US 2982736A US 2982736D A US2982736D A US 2982736DA US 2982736 A US2982736 A US 2982736A
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- United States
- Prior art keywords
- sulfuric acid
- reaction
- wetting agent
- weight
- sulfonic acids
- Prior art date
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- 238000005406 washing Methods 0.000 title description 6
- 238000006243 chemical reaction Methods 0.000 claims description 66
- 239000000080 wetting agent Substances 0.000 claims description 66
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 62
- 239000007788 liquid Substances 0.000 claims description 62
- 230000001737 promoting Effects 0.000 claims description 56
- 239000000463 material Substances 0.000 claims description 54
- 239000000203 mixture Substances 0.000 claims description 34
- 239000003599 detergent Substances 0.000 claims description 32
- 230000002378 acidificating Effects 0.000 claims description 30
- 229910010272 inorganic material Inorganic materials 0.000 claims description 30
- 239000011147 inorganic material Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 26
- 239000007787 solid Substances 0.000 claims description 16
- 210000004940 Nucleus Anatomy 0.000 claims description 10
- 150000001298 alcohols Chemical class 0.000 claims description 8
- 150000002334 glycols Chemical class 0.000 claims description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 239000011541 reaction mixture Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 230000001264 neutralization Effects 0.000 claims description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-M bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 6
- 101700018994 ARYL Proteins 0.000 claims 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N Diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 36
- -1 alkyl aryl sulfonic acids Chemical class 0.000 description 34
- 239000002253 acid Substances 0.000 description 26
- 229940032330 Sulfuric acid Drugs 0.000 description 24
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 22
- 239000011734 sodium Substances 0.000 description 22
- 229910052708 sodium Inorganic materials 0.000 description 22
- 235000019441 ethanol Nutrition 0.000 description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- HVWGGPRWKSHASF-UHFFFAOYSA-N octadecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCCCCCCCOS(O)(=O)=O HVWGGPRWKSHASF-UHFFFAOYSA-N 0.000 description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M NaHCO3 Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 12
- 239000004115 Sodium Silicate Substances 0.000 description 12
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 12
- 235000019832 sodium triphosphate Nutrition 0.000 description 12
- KWXICGTUELOLSQ-UHFFFAOYSA-N 4-Dodecylbenzenesulfonic Acid Chemical compound CCCCCCCCCCCCC1=CC=C(S(O)(=O)=O)C=C1 KWXICGTUELOLSQ-UHFFFAOYSA-N 0.000 description 10
- 125000004432 carbon atoms Chemical group C* 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- KWKXNDCHNDYVRT-UHFFFAOYSA-N Dodecylbenzene Chemical compound CCCCCCCCCCCCC1=CC=CC=C1 KWKXNDCHNDYVRT-UHFFFAOYSA-N 0.000 description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N Sodium silicate Chemical class [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 8
- 239000001913 cellulose Substances 0.000 description 8
- 229920002678 cellulose Polymers 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 235000019795 sodium metasilicate Nutrition 0.000 description 8
- 229910052911 sodium silicate Inorganic materials 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 150000007513 acids Chemical class 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 239000004615 ingredient Substances 0.000 description 6
- 150000004686 pentahydrates Chemical class 0.000 description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 6
- 235000017550 sodium carbonate Nutrition 0.000 description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000001488 sodium phosphate Substances 0.000 description 6
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 6
- HENIRSYLRPFZAW-UHFFFAOYSA-N 2-(2-hydroxyethoxy)ethanol;sulfuric acid Chemical compound OS(O)(=O)=O.OCCOCCO HENIRSYLRPFZAW-UHFFFAOYSA-N 0.000 description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N Oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 4
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 125000005233 alkylalcohol group Chemical group 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- QPXWUAQRJLSJRT-UHFFFAOYSA-N diethoxyphosphinothioyl diethyl phosphate Chemical compound CCOP(=O)(OCC)OP(=S)(OCC)OCC QPXWUAQRJLSJRT-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 4
- 235000019351 sodium silicates Nutrition 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 235000019801 trisodium phosphate Nutrition 0.000 description 4
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 4
- 238000009736 wetting Methods 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 241000158728 Meliaceae Species 0.000 description 2
- 210000001178 Neural Stem Cells Anatomy 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- 210000003491 Skin Anatomy 0.000 description 2
- LEHOTFFKMJEONL-UHFFFAOYSA-N Trioxopurine Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 description 2
- 229940116269 Uric Acid Drugs 0.000 description 2
- HDFXRQJQZBPDLF-UHFFFAOYSA-L [Na+].[Na+].OC([O-])=O.OC([O-])=O Chemical compound [Na+].[Na+].OC([O-])=O.OC([O-])=O HDFXRQJQZBPDLF-UHFFFAOYSA-L 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K [O-]P([O-])([O-])=O Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 125000002877 alkyl aryl group Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000003247 decreasing Effects 0.000 description 2
- LDMOEFOXLIZJOW-UHFFFAOYSA-N dodecane-1-sulfonic acid Chemical compound CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 description 2
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 2
- 229940093476 ethylene glycol Drugs 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
- 125000000267 glycino group Chemical group [H]N([*])C([H])([H])C(=O)O[H] 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006011 modification reaction Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 238000007788 roughening Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N silicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 239000001187 sodium carbonate Substances 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 235000011008 sodium phosphates Nutrition 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N sulfonic acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- 150000003460 sulfonic acids Chemical class 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 150000007968 uric acids Chemical class 0.000 description 2
Definitions
- inorganic alkaline material By spraying an excess of inorganic alkaline material with the synthetic organic, acidic wetting agent, some of the inorganic alkaline material will remain unreacted after all the organic wetting agent has been neutralized.
- the excess unreacted alkaline material serves as an inorganic detergent builder. This process may becarried out in a closed, horizontally extendingreaction vessel having horizontally rotating mixing paddles therein v liquid, a free-flowing product will not be produced, iustead a discolored (i'.e., brown) gummy mass will result;
- the reaction promoting liquid thus serves to enable the acidic Wetting agent to promptly'and' complet l react with the" inorganic alkaline material to form solid, -free-fiowing particles having improved detergency and obviates" the need for a drying step.
- the reaction between the inorganic alkaline detergent and acid etting agent will continue over an extended period of time which may .e nc ompass several days or more, whereas complete neutralizationmay be eliected in our proces in about 3-5 minutes.- i
- liquids may be used,'such"as ethyl alcohol, rretliyl'ia' lco hol, isopr'o'pyl alcohoLjbutyl alcohol, .ethyleneglycol, diethylene glycol, propylene,gly' gg'ol, and, 'other1similar water-soluble organicc'ompounds, wl iich increalse the realc and/or su tur caqi s to p wetting agent, 7 comprises: spraying i solid particulate Linaction between the -synthetic;organ-1 tion having.
- reaction promotingliquid includes glycols
- the synthetic organic wetting agent is restricted to member of the class consisting of higher 'alkyl aryl sulforiic acids, higher alkyl sulfonic acids, higher alkyl sul- ⁇ uric acid esters, and admixtures thereof.
- wetting agents include dodecyl benzene sulfonic acid, mahogany acids, octadecyl sulfuric acid ester, lauryl sulfuric acid ester, .dodecyl sulfonic acid, and the like.
- the inorganic alkaline .material serves to neutralize the synthetic organic, acidic wetting.
- This alkaline material may include such inorganic alkalies as caustic, sodium carbonate, sodium tripolyphosphate, sodium silicates,,sodium bicarbonate, any of the other alkalies employed in the detergent field, and admixtures thereof.
- the following samples are typical particulate detergent compositions of this invention which employ a sulfonic acid as the synthetic organic, acidic wetting agent.
- An admixture of the wetting agent and reaction promoting liquid were sprayed on the particulate inorganic material.
- PromotlngLlquid Sulfuri Acid Particulate Inorganic Material Perce Soda Ash Light Na Om) 59. 27 Sodium 'Iripolyp osphetecarboxymethyl Celluvant;
- Particulate Inorganic Materiel Soda Ash, Light 54.00 A 54. 00 Sodium Carboxymcthyl Cellulose l. 00 1.00 Wetting Agent:
- Typical formulations of this invention employing a suluric acid ester which have been prepared successfully in accordance with the new method of this invention and which serve as excellent detergents are Samples Particulate Inorganic Material: Percent Soda Ash, Light NSC/Q3) 59.
- g-go 9: 9 09 go Formulations containing substantially the same ingredicuts and portions as those of Samples 1, 3, 5, 7, 9, .11, 13, and 20-26 were prepared except that in each case ethyl alcohol was employed in place of the diethylene glycol reaction promoting liquid.
- the resulting coating about the nucleus of particulate alkaline material did not retain the reaction promoting liquid since the ethyl alcohol was evaporated by the heat of reaction.
- laurylsulfuric acid ester was substituted for oc'tadecyl sulfuric acid ester.
- Formulations were also prepared which containedsubstantially the same ingredients as Samples 1, 13, 20 and 26, except that the indicated levels of wetting agent conthe acidic wetting agent.
- the level of synthetic organic, acidic wetting agent may be at low as 0.5% by weight of the reaction mixture and as high as about 45-50% by weight of said.mixture.
- a particulate detergent composition consisting essentially of a nucleus of inorganic material and a coating of a relatively neutral, reaction-set salt of a synthetic organic, acidic Wetting agent, which comprises: spraying solid particulate inorganic alkaline material which serves as a detergent builder with about 05-50% by weight, based on the weight of the reaction mixture, of a substantially anhydrous normally slow-reacting member of the class consisting of higher alkyl aryl sulfonic acids, higher .alkyl sulfonic acids, higher alkyl sulfuric acid esters, the alkyl groups in said sulfonic acids and said sulfuric acid esters containing about 12-18 carbon atoms and admixtures thereof in the presence of at least about 20% by weight, based on the Weight of said reacting members, of a substantially anhydrous reaction promoting liquid consisting essentially of a member of the group consisting of lower alkylene glycols having about 2-4 carbon atoms, lower alkyl
- reaction promoting liquid is concentrated sulfuric acid.
- reaction promoting liquid is a lower alkylene glycol having about 2-4 carbon atoms.
- reaction promoting liquid is diethylene glycol
- reaction promoting liquid is propylene glycol
- reaction promoting liquid is a lower alkyl alcohol having about 1-4 carbon atoms.
- said inorganic alkaline material consists essentially of at least one member of the group consisting .of caustic soda, soda ash, sodium silicates, sodium bicarbonate, and sodium phosphates.
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- Detergent Compositions (AREA)
Description
I .nuc leuslof inorganic material and a coatingof k V Ineutral,- reaction:set sa lt 9f asynthetic organic, acidic United States Patent METHOD OF PREPARING WASH ING COMPOSITION Vladimir Dvorkovitz, Kansas City, Mo., and Jerome Arthur Goldman, Evanston, Ill., assignors to The Diversey Corporation, Chicago, Ill., a corporation of Illinois No Drawing, Filed 'Aug. 13, 1957, Ser. No. 677,853
8 Claims. ,(Cl. 2 52-4138 ganic alkaline material with a normally slow-reacting member of the classconsisting of higher alkyl aryl sulfonic acids, higher alkyl sulfonic acids, higher alkyl sulfuric acid esters, and admixtures thereof in the presence of a small amount of reaction promoting liquid, whereby said member is completely reacted with said alkaline material and a dry, solid, coated, finely divided detergent composition is produced at once'during the neutralization reaction. 7
The term normally; slow-reacting herein refers to the fact that when the particulate alkaline material is sprayed with the acidic wetting agent, in the above pro cess,'in the absence of the reaction promoting liquid, the wetting'agent slowly reacts with the alkalinematerial.
This application is a continuation-impart of our copending application Serial No. 427,677, filed May 4, l954, now abandoned, which, in .turn, was a continuation-in-part'of our copending applicationSeria-l No. 348,- 512, filed Ap i 1953; ne .Qbfilldpmd. Although synthetic organic, acidic wetting agents from the :class consisting of higher alkyl aryl sulfonic acids, higher alkyl sulfonic ,acids, higher alkyl sulfonicacid "ice ing member of the class consisting of higher alkyl aryl sulfonic acids, higher alkyl sulfuric acid esters, higher alkyl sulfonic acids, and admixtures thereof in the presence of a small amount of reaction promoting liquid '(e.g.,.glyco1, alcohol, sulfuric acid), whereby said memher is completely reacted with the alkaline material and a dry, solid, coated, finely divided detergent composition is produced atonce during the neutralization reaction. By spraying an excess of inorganic alkaline material with the synthetic organic, acidic wetting agent, some of the inorganic alkaline material will remain unreacted after all the organic wetting agent has been neutralized. The excess unreacted alkaline material serves as an inorganic detergent builder. This process may becarried out in a closed, horizontally extendingreaction vessel having horizontally rotating mixing paddles therein v liquid, a free-flowing product will not be produced, iustead a discolored (i'.e., brown) gummy mass will result;
and a stationary, horizontally extending, overhead pipe with spray nozzles which spray the liquid material on to the alkaline material. It is preferable to premix the reaction promoting liquid with the acidic wetting agent, although each of these constituents may be separately applied to the particulate alkaline material.
The reaction promoting liquid thus serves to enable the acidic Wetting agent to promptly'and' complet l react with the" inorganic alkaline material to form solid, -free-fiowing particles having improved detergency and obviates" the need for a drying step. In the event the inorganic alkalinematerial is sprayed with the organic acid material in the absence of the reaction-promoting in addition, the reaction between the inorganic alkaline detergent and acid etting agent will continue over an extended period of time which may .e nc ompass several days or more, whereas complete neutralizationmay be eliected in our proces in about 3-5 minutes.- i
V a Our process produces a Washing composition that is in thecform of finely divided particles, each of which comprises a nucleus of inorganic alkaline material surrounded by the neutralized reaction product i.e.-, salt) produced by the interaction of theacidicwetting agent esters, and admixtures thereof have some detergent propreaqti on products must be dried (e.g.,"in drum dryers) in order to volatilize the water. After such products. are
dried, they must be ground in order to producea finely' divided, free flowing detergent 'product. 1 'We have discovered a process by which the normally slow-reacting synthetic organic, acidic wetting agent rapidly and completely reacts with the inorganic alkaline material t harm a parti ulate .compcsitiofi rwit q ti I quiring eithera separate'drying step or grindingthe 7 reaction product. This heterogeneous process for pro- 'ducing a particulate" detergentcomposition havingwa,
e t ie i.
withv-aiportion'of the alkaline material. Thus, the pH of the particles as a whole ismarkedly in excess of the" H sl za isstiss .srea t eo Thi Q nables the particles tojbe added to waterto form a soluon to the particulate alkaline materiaL. For example, liquids may be used,'such"as ethyl alcohol, rretliyl'ia' lco hol, isopr'o'pyl alcohoLjbutyl alcohol, .ethyleneglycol, diethylene glycol, propylene,gly' gg'ol, and, 'other1similar water-soluble organicc'ompounds, wl iich increalse the realc and/or su tur caqi s to p wetting agent, 7 comprises: spraying i solid particulate Linaction between the -synthetic;organ-1 tion having. a .pH below about 8 during the period that the, particles are being hand agitated in-thefvvate'riand are in direct contact with the skin: Under conditions, subsequent roughe ning and ehapping-. of the hands are lessened. g x l The term reaction promotingliquid includes glycols,
alcohols, sulfuricacidandadmixtures thereof, whiiihlmay be sprayed with the synthetic organid acidic wettiugagent 's s t f hwartin asse w kthe p iu lkali'ne material. We prefer toemploy fd th der Propy yc rathenthanrolaftileji mate to minimize tire hazards. Although minor-amounts of j water as well as admixtures of was? ths wl sad .21:
and theIalkaline material'," thejus'e of water req careful controls,-since excessiveleyels thereof a formation of a gummy undivided mass; on the other hand, alcohols, glycols, and sulfuric acid do not require such careful control of the levels used. Thus, water is clearly distinguishable from the glycols, alcohols, sul furic acid, or aqueous dilutionsthereof, and its use is restricted to corlditionswhich permit very careful control of the level present inthe mix of alkaline material and synthetic organic, acidic wetting agent.
The synthetic organic wetting agent is restricted to member of the class consisting of higher 'alkyl aryl sulforiic acids, higher alkyl sulfonic acids, higher alkyl sul- {uric acid esters, and admixtures thereof. For example, such wetting agents include dodecyl benzene sulfonic acid, mahogany acids, octadecyl sulfuric acid ester, lauryl sulfuric acid ester, .dodecyl sulfonic acid, and the like. The inorganic alkaline .material serves to neutralize the synthetic organic, acidic wetting. agent and the excess um'eacted portion, which constitutesthe nucleus of our particulatedetergent composition, serves as a detergent builder. I This alkaline material may include such inorganic alkalies as caustic, sodium carbonate, sodium tripolyphosphate, sodium silicates,,sodium bicarbonate, any of the other alkalies employed in the detergent field, and admixtures thereof.
The following samples are typical particulate detergent compositions of this invention which employ a sulfonic acid as the synthetic organic, acidic wetting agent. An admixture of the wetting agent and reaction promoting liquid were sprayed on the particulate inorganic material.
Samples Particulate Inorganic MaterialL Wettin Agent:
Reaction. PromotlngLlquid Sulfuri Acid Particulate Inorganic Material: Perce Soda Ash Light Na Om) 59. 27 Sodium 'Iripolyp osphetecarboxymethyl Cellulosen;
Wetting Agent:
Dodecylbenzene Sulfonic Acid Reaction Promoting Liquid:
Sulfuric Acid Diethylene Glycol Percent N W r 9 5 Particulate Inorganic Materiel:
Soda Ash,'Light Sodium Bicarbonate.
Sodium Tripolyphosphate Wetting Agent; I V Dodecylbenzene Suli'onic Acid Reaction Promoting Liquid: a
S or Acid I 'Dicthylene G1yeol.
Particulate Inorganic Material- Soda. Light; Trisodium Phosphate, Sodium Metasilicate Pentahydrete...
- G Silicate (high SiO 'to N820 (content).'.
Wetting Agent:
Dodecylbenzene Suli'onic Acid Reaction Promoting Liquid: I
Sulfuric Acid U Diethylene Glycol NNNCO IN H DOOM H (O pa e-- Tetrasodium Pyrophos hate; Trisodium Phosphate, ines Sodium Metasilicete Pentahydrate Olate Flakes (oleic acid-containing soap) Soda Ash, Light Wetting Agent:
.Dodecylbenzene Sulfonic Acid Reactiltlifn'lromoting Liquid:
S uric Acid -Diethy1ene Glycol rteo: :noocio N on -10 lmooco on no Particulete Inorganic Materiah Soda Ash, Light--. Sodium Bicarbonat Sodium Tripolyphosphato,
l Do ecylbenzeneSulionic Acid... H
0 Diethylene Glycol Samples Particulate Inorganic Material: 7 Percent Percent Sodium Tripolyphosphcte, Gran a. 22. Sodium Metasilicate Pentahydrate, Gran.. 16.00 16. 00 Oarboxymethyl Cellulose, Low Viscosity (Hercules 0'1 Grade) 0. 23 0.23 Soda Ash, Dense 48. 27 4B. 27 Soda Ash, Light 10.00 10.00 Wetting Agent: i
Dodecylbenzene Sulfonic Acid 2. 38 1 12 Reaction'Promoting Liquid:
Sulfuric Acid 0. 42 1.08 Diethylene Glycol 0. 70 0.70
Particulate Inorganic Material:
Sodium Tripolyphosphate, Gran 10.00 10. 00 Soda Ash, Dense..- 65. 00 65. 00 Soda Ash, Light 20.00 20.00 Wetting Agent:
Dodecylbenzene Sulfonic Acid 3. 40 1.60 Reaction Promoting Liquid: 1 I
Sulfuric Acid 0. 60 2. 40 Diethylene Glycol 1.00 1.00
Particulate Inorganic Material Sodium Tri 10.00 Soda Ash, Light 65.00 Wetting Agent:
Dodecylbenzene Sulionic Acid 10.00 Reaction Promoting Liquid:
Sulfuric Acid 16.00
Particulate Inorganic Material;
Sodium Tripolyphosphate, Gran 10. 00. 10.00 Soda Ash, ight. 55.00 55. 00 .Wetting Agent: v y Dodecylbenzene Sulfonic Acid 25. 12 00 Reaction Promoting Liquid:
Sulfuric Acid 4. 50 18. 00 Ethyl Alcohol 6. 00 5. 00
Particulate Inorganic Materiel: Soda Ash, Light 54.00 A 54. 00 Sodium Carboxymcthyl Cellulose l. 00 1.00 Wetting Agent:
Dodecylbenzene Sulfonlc Acid 34. 00 16.00 Reaction Promoting Liquid: 7
Sulfuric Acid... 0.00 24.00 Ethyl Alcohol 5.00 5. 00
Typical formulations of this invention employing a suluric acid ester which have been prepared successfully in accordance with the new method of this invention and which serve as excellent detergents are Samples Particulate Inorganic Material: Percent Soda Ash, Light NSC/Q3) 59.
Sodium Tripolyp osphate... 28.00 Oerboxymethyl Cellulose 0.23 Wetting Agent:
Octadecyl sulfuric acid ester. 8. 50 Reaction Promoting Liquid:
Sulfur c 1 50 Diethylene Glycol 2-50 Particulate Inorganic Material:
Soda. Ash, Light Sodium Bicarbonate Sodium Metasllicate Pentahydrate" Sodium Tripoiyphosphate Wetting Agent:
. Octadecyl sulfuric acid ester Reaction Promoting Liquid:
' Sulfuric Acid i Diethylene Glycol 1 v Sulfuric Acid-- Diethylene Glycol........................................
Samples Particulate Inorganic Material:
Tetrasedium Pyrophos hate Trisodrum Phosphate, ines Sodium Metasilicate Pentahydrate Olate Flakes Soda Ash, Li ht Wetting Agent:
Octadecyl sulfuric acid ester Reaction Promoting Liquid:
uliurie Acid. Diethylene Glyml Percent to P9 2*.9 \rus co moo one on 000 Particulate Inorganic Material:
Soda Ash, Li ht Sodium Bicar Sodium Tripolyphosphate, Gran 15.00 Wetting Agent:
Octadecyl sulfuric acid ester Reaction Promoting Liquid:
Sulfuric Acid 0. 63 Diethylene Glyr-nl 0.20
Particulate Inorganic Material:
Sodium Tripolyphosphate, Gran Sodium Metasilicate Pentahydrate, Gran OaGrbozymethyl Cellulose, Low Viscosity (Hercules 0'1 ra Soda Ash, Dense Soda Ash, Li ht Wetting Agent:
Octadecyl sulfuric acid ester Reaction Promoting Liquid:
111111110 Avid Diethylene Glyml Particulate Inorganic Material:
Sodium Trlpolyphosphate, Gran Soda Ash, Dense Soda Ash, Tiirr'l'lf Wetting Agent:
Octadecyl sulfuric acid ester Reaction Promoting Liquid:
Sulfuric Acid- Diet-hylene Glyml to wona:
g-go 9: 9 09 go Formulations containing substantially the same ingredicuts and portions as those of Samples 1, 3, 5, 7, 9, .11, 13, and 20-26 were prepared except that in each case ethyl alcohol was employed in place of the diethylene glycol reaction promoting liquid. The resulting coating about the nucleus of particulate alkaline material did not retain the reaction promoting liquid since the ethyl alcohol was evaporated by the heat of reaction.
Formulations were prepared which contained the same ingredients and proportions of Samples 20-26, however,
laurylsulfuric acid ester was substituted for oc'tadecyl sulfuric acid ester.
' Formulations were also prepared'which contained substantially the same ingredients and proportions as those,
of Samples 20-26, Withthe exception that the levels of wetting agent were decreased 53% of the indicated values and the levels of sulfuric acid were increased 300% of the indicated values. v
Formulations were also prepared which containedsubstantially the same ingredients as Samples 1, 13, 20 and 26, except that the indicated levels of wetting agent conthe acidic wetting agent. The level of synthetic organic, acidic wetting agent may be at low as 0.5% by weight of the reaction mixture and as high as about 45-50% by weight of said.mixture.
The foregoing detailed description has been given for clearness of understanding only, and no unnecessary limitations should be understood therefrom, as modifications will be obvious to those skilled in the art.
We claim:
1. The processof producing a particulate detergent composition consisting essentially of a nucleus of inorganic material and a coating of a relatively neutral, reaction-set salt of a synthetic organic, acidic Wetting agent, which comprises: spraying solid particulate inorganic alkaline material which serves as a detergent builder with about 05-50% by weight, based on the weight of the reaction mixture, of a substantially anhydrous normally slow-reacting member of the class consisting of higher alkyl aryl sulfonic acids, higher .alkyl sulfonic acids, higher alkyl sulfuric acid esters, the alkyl groups in said sulfonic acids and said sulfuric acid esters containing about 12-18 carbon atoms and admixtures thereof in the presence of at least about 20% by weight, based on the Weight of said reacting members, of a substantially anhydrous reaction promoting liquid consisting essentially of a member of the group consisting of lower alkylene glycols having about 2-4 carbon atoms, lower alkyl alcohols having about 1-4 carbon atoms, concentrated sulfuric acid, and admixtures thereof, whereby said member is completely reacted with said alkaline material during a period of up to about 5 minutes and a dry, solid, coated, finely divided detergent composition is produced at once during the neutralization reaction.
2. The process of claim 1 wherein the reaction promoting liquid is concentrated sulfuric acid.
3. The process of claim 1 wherein the reaction promoting liquid is a lower alkylene glycol having about 2-4 carbon atoms.
4. The process of claim 1 wherein the reaction promoting liquid is diethylene glycol.
5. The process of claim 1 wherein the reaction promoting liquid is propylene glycol.
6. The process of claim 1 wherein the reaction promoting liquid is a lower alkyl alcohol having about 1-4 carbon atoms.
p 7. The process of claim 1 wherein said inorganic alkaline material consists essentially of at least one member of the group consisting .of caustic soda, soda ash, sodium silicates, sodium bicarbonate, and sodium phosphates.
8. The process of claim 1 wherein said inorganic alkaline material contains soda ash.
References Cited in the file of this patent UNITED STATES PATENTS 1,989,765 Moss p Feb. 5, 2,243,054 .Vail May 20, 1941 2,287,864 I Burton June, 30, 1942 2,351,559. Treflder" June 13, 1944 2,356,443 ',Bissinger Aug. 22, 1944 2,390,406 Wegst etal. 'Dec. 4, 1945 2,465,346 -Bodman Mar. 29, 1949 2,730,507 Bradford. Jan. 10, 1956 2,766,276 Kolling Oct. 9, 1956 2,767,146 I Bonewitz et a1. Oct. 16, 6 2,776,943 Eaton Jan. 8, 1957 4 2,791,562 1957 UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent No, $982,736 I May 2, 1961 Vladimir Dvorkovitz et al.
It is hereby certified that error appears in the above numbered patent requiring correction and that the said Letters Patent. should read as "corrected below.
Column 6, line 24 for "members" read member Signed and sealed this 19th day of September 1961.,
(SEAL) Attest:
ERNEST W. SWIDER DAVID L. LADD Attesting Officer Commissioner of Patents
Claims (1)
1. THE PROCESS OF PRODUCING A PARTICULATE DETERGENT COMPOSITION CONSISTING ESSENTIALLY OF A NUCLEUS OF INORGANIC MATERIAL AND COATING OF A RELATIVELY NEUTRAL, REACTION-SET SALT OF A SYNTHETIC ORGANIC, ACIDIC WETTING AGENT, WHICH COMPRISES: SPRAYING SOLID PARTICULATE INORGANIC ALKALINE MATERIAL WHICH SERVES AS A DETERGENT BUILDER WITH ABOUT 0.5-50% BY WEIGHT, BASED ON THE WEIGHT OF THE REACTION MIXTURE, OF A SUBSTANTIALLY ANHYDROUS NORMALLY SLOW-REACTING MEMBER OF THE CLASS CONSISTING OF HIGHER ALKYL ARYL SULFONIC ACIDS, HIGHER ALKYL SULFONIC ACIDS, HIGHER ALKYL SULFURIC ACID ESTERS, THE ALKYL GROUPS IN SAID SULFONIC ACIDS AND SAID SULFURIC ACID ESTERS CONTAINING ABOUT 12-18 CARBON ATOMS AND ADMIXTURES THEREOF IN THE PRESENCE OF AT LEAST ABOUT 20% BY WEIGHT, BASED ON THE WEIGHT OF SAID REACTING MEMBERS, OF A SUBSTANTIALLY ANHYDROUS REACTION PROMOTING LIQUID CONSISTING ESSENTIALLY OF A MEMBER OF THE GROUP CONSISTING OF LOWER ALKYLENE GLYCOLS HAVING ABOUT 2-4 CARBON ATOMS, LOWER ALKYL ALCOHOLS HAVING ABOUT 1-4 CARBON ATOMS, CONCENTRATED SULFURIC ACID, AND ADMIXTURES THEREOF, WHEREBY SAID MEMBER IS COMPLETELY REACTED WITH SAID ALKALINE MATERIAL DURING A PERIOD OF UP TO ABOUT 5 MINUTES AND A DRY, SOLID, COATED, FINELY DIVIDED DETERGENT COMPOSITION IS PRODUCED AT ONCE DURING THE NEUTRALIZATION REACTION.
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| Publication Number | Publication Date |
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| US2982736A true US2982736A (en) | 1961-05-02 |
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ID=3449926
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US2982736D Expired - Lifetime US2982736A (en) | Method of preparedg washing |
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| US (1) | US2982736A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3178370A (en) * | 1963-02-27 | 1965-04-13 | Procter & Gamble | Milled detergent bar |
| US3367831A (en) * | 1965-03-25 | 1968-02-06 | Sidney J.M. Walker | Method for treating animals infested with pests of the phylum arthropoda |
| US3472784A (en) * | 1966-09-30 | 1969-10-14 | Monsanto Co | Detergent process |
| DE2203552A1 (en) * | 1971-02-01 | 1972-08-10 | Colgate Palmolive Co | Neutralization process for surfactants in acidic form |
| US6096703A (en) * | 1996-07-31 | 2000-08-01 | The Procter & Gamble Company | Process and composition for detergents |
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| US1989765A (en) * | 1930-06-25 | 1935-02-05 | Swann Res Inc | Sodium meta silicate detergent |
| US2243054A (en) * | 1937-11-27 | 1941-05-20 | Philadelphia Quartz Co | Detergent composition and manufacture thereof |
| US2287864A (en) * | 1940-10-28 | 1942-06-30 | Heyden Chemical Corp | Beta oxy naphthoic acid and process for preparing the same |
| US2351559A (en) * | 1944-06-13 | Process for the preparation of | ||
| US2356443A (en) * | 1940-07-16 | 1944-08-22 | Drew Associates Inc | Method of making a composition for use in detergents |
| US2390406A (en) * | 1943-07-17 | 1945-12-04 | Wyandotte Chemicals Corp | Alkaline composition of matter |
| US2465346A (en) * | 1943-07-15 | 1949-03-29 | Lever Brothers Ltd | Dedusting process and product thereof |
| US2730507A (en) * | 1952-01-28 | 1956-01-10 | Swift & Co | Method of making dustless soap powder |
| US2766276A (en) * | 1951-04-25 | 1956-10-09 | Ruhrchemie Ag | Neutralization of sulfonic acids |
| US2767146A (en) * | 1956-10-16 | Method of making cleaning | ||
| US2776943A (en) * | 1951-05-14 | 1957-01-08 | Procter & Gamble | Treatment of soap particles |
| US2791562A (en) * | 1957-05-07 | Method of producing dry detergent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2351559A (en) * | 1944-06-13 | Process for the preparation of | ||
| US2767146A (en) * | 1956-10-16 | Method of making cleaning | ||
| US2791562A (en) * | 1957-05-07 | Method of producing dry detergent | ||
| US1989765A (en) * | 1930-06-25 | 1935-02-05 | Swann Res Inc | Sodium meta silicate detergent |
| US2243054A (en) * | 1937-11-27 | 1941-05-20 | Philadelphia Quartz Co | Detergent composition and manufacture thereof |
| US2356443A (en) * | 1940-07-16 | 1944-08-22 | Drew Associates Inc | Method of making a composition for use in detergents |
| US2287864A (en) * | 1940-10-28 | 1942-06-30 | Heyden Chemical Corp | Beta oxy naphthoic acid and process for preparing the same |
| US2465346A (en) * | 1943-07-15 | 1949-03-29 | Lever Brothers Ltd | Dedusting process and product thereof |
| US2390406A (en) * | 1943-07-17 | 1945-12-04 | Wyandotte Chemicals Corp | Alkaline composition of matter |
| US2766276A (en) * | 1951-04-25 | 1956-10-09 | Ruhrchemie Ag | Neutralization of sulfonic acids |
| US2776943A (en) * | 1951-05-14 | 1957-01-08 | Procter & Gamble | Treatment of soap particles |
| US2730507A (en) * | 1952-01-28 | 1956-01-10 | Swift & Co | Method of making dustless soap powder |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3178370A (en) * | 1963-02-27 | 1965-04-13 | Procter & Gamble | Milled detergent bar |
| US3367831A (en) * | 1965-03-25 | 1968-02-06 | Sidney J.M. Walker | Method for treating animals infested with pests of the phylum arthropoda |
| US3472784A (en) * | 1966-09-30 | 1969-10-14 | Monsanto Co | Detergent process |
| DE2203552A1 (en) * | 1971-02-01 | 1972-08-10 | Colgate Palmolive Co | Neutralization process for surfactants in acidic form |
| US6096703A (en) * | 1996-07-31 | 2000-08-01 | The Procter & Gamble Company | Process and composition for detergents |
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