US3676352A - Process for the manufacture of enzyme and perborate-containing detergent compositions - Google Patents

Process for the manufacture of enzyme and perborate-containing detergent compositions Download PDF

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Publication number
US3676352A
US3676352A US5945A US3676352DA US3676352A US 3676352 A US3676352 A US 3676352A US 5945 A US5945 A US 5945A US 3676352D A US3676352D A US 3676352DA US 3676352 A US3676352 A US 3676352A
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US
United States
Prior art keywords
acid
builder
enzyme
sodium
weight percent
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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.)
Expired - Lifetime
Application number
US5945A
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English (en)
Inventor
Dieter Grimm
Joachim Kandler
Karl Merkenich
Wolf-Dieter Pirig
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Knapsack AG
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Knapsack AG
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Publication of US3676352A publication Critical patent/US3676352A/en
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Classifications

    • 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
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
    • C11D3/38672—Granulated or coated enzymes
    • 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
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
    • C11D3/38609—Protease or amylase in solid compositions only

Definitions

  • Solid detergent components comprising a powder mixture consisting substantially of one or more alkali metal salts as a builder substance and sodium perborate are fluidized by means of air and the fluidized powder mixture is granulated by spraying liquid detergent components comprising water or an aqueous solution or suspension of one or more binders and optionally a surface-active substance, onto it.
  • the enzyme may be present in the powder mixture or in the water or aqueous solution or suspension to be sprayed thereonto.
  • the present invention relates to a process for the manufacture of detergent compositions containing enzymes and perborates, which comprises spraying liquid or pasty detergent components onto solid, powdery and air-fluidized detergent components with the resultant formation of a granulated detergent composition having good flow properties.
  • the fine-powdered enzyme be granulated by means of water and adhered to a carrier of good flowability, suitable for use as a detergent component.
  • the water can, for example, be sprayed onto the solid detergent components.
  • the carriers suggested to be used include anhydrous or partially hydrated sodium tripolyphosphate, or a granulate made therefrom together with, for example, sodium carboxymethylcellulose, corrosion inhibitors, optical brighteners or perfumes.
  • the water used for adhering the enzyme to the carrier is employed in a quantity sufficient to simultaneously hydrate at most 90 percent of the carrier. The granulated matter so made has been found to have a satisfactory flowability.
  • South African Pat. No. 67/2415 describes a process for the manufacture of free-flowing, enzyme-containing granulated detergents, wherein the surface of the granulated base detergent, for example sodium tripolyphosphate or sodium perborate, is first rendered glutinous by blending it with a low melting, non-ionic surface-active material, and the granulated particles are then powdered or dusted with fine-powdered enzyme.
  • a preferred feature of this process comprises using a blend of base detergent and enzyme powder, spraying the surface-active substance, which is liquefied by heating it, onto the blend with thorough agitation, and thereby adhering the enzyme to the base detergent.
  • the useful enzymes include hydrolases, such as proteases, esterases, carbohydrases or nucleases, and the useful surface-active substances include, for example, polyethylene glycol or polyoxymethylene glyceride esters. This dusting process produces granulated matter having a considerable proportion of small granulate particles therein. This is undesirable in the production of detergents as the flowability of the detergent is reduced thereby.
  • a further process for the manufacture of a biologically active and perborate containing detergent has been reported in South-African Pat. No. 67/2413 which comprises first spraydrying sodium tripolyphosphate and enzyme so as to obtain a granulate and then dry-blending the granulate with sodium perborate, a granulate composition of further detergent components, such as sodium silicate, carboxymethylcellulose and a surface-active substance.
  • the present invention now provides a single step process for the manufacture of granulated, biologically -active and perborate-containing detergent compositions which combine free flow properties with freedom from dust and further combine a uniform particle size with a constant apparent density.
  • the process of the present invention for the manufacture of enzyme and perborate-containing detergent compositions by spraying liquid or pasty detergent components onto solid, powdery detergent components with the resultant formation of a readily flowable granulate comprises more particularly air-fluidizing the solid detergent components comprising a powder mixture consisting substantially of one or more alkali metal salts as a builder substance and sodium perborate, the cation of the alkali metal salt being a lithium, sodium, potassium or ammonium ion, and the acid salt component being sulfuric acid, silicic acid, disilicic acid, carbonic acid, an oligo or polyphosphoric acid, nitrilotriacetic acid, ethylenediaminetetracetic acid, a homopolymer or copolymer of an unsaturated aliphatic polycarboxylic acid, a copolymer of an unsaturated aliphatic polycarboxylic acid with an alkylene, an unsaturated monocarboxylic acid or a further vinyl compound, a copolymer
  • the builder substance is sodium tripolyphosphate with a phase-l-content of between 20 and 100, preferably 40 and 80, weight percent, or sodium pyrophosphate, sodium hexametaphosphate, trisodium nitrilotriacetate or tetrasodium ethylenediaminetetracetate.
  • a further preferred feature comprises using sodium tripolyphosphate having an apparent density of more than 550 grams/liter, preferably between about 600 and 700 grams/liter.
  • Biologic activity can be imparted to the detergent composition of the present invention by means of a wide variety of enzymes, such as hydrolases, oxidoreductases, transferases, desmolases or isomerases, bacterial proteases being preferred.
  • enzymes such as hydrolases, oxidoreductases, transferases, desmolases or isomerases, bacterial proteases being preferred.
  • the detergent composition of the present invention may contain further solid addends, for example perfumes, optical brighteners, desinfectants and peroxide stabilizers or activators, such as alkaline earth metal silicates, heavy metal salts or tetracetylethylene diamine.
  • solid addends for example perfumes, optical brighteners, desinfectants and peroxide stabilizers or activators, such as alkaline earth metal silicates, heavy metal salts or tetracetylethylene diamine.
  • Tylose is preferably used as the cellulose ether.
  • the granulating step should conveniently be carried out with the use of a quantity of water sufficient to effect granulation of the builder. Between about 2 and 50 weight percent water, based on the builder, should conveniently be used to efiect hydration. In those cases in which the builder is sodium tripolyphosphate having a phase-I-content of between 20 and 100 weight percent, where the water is found to effect transformation into the hexahydrate, it is advantageous to use the water at a rate of between about 2 and 30 weight percent, based on the sodium tripolyphosphate.
  • the detergent composition should conveniently contain between 20 and 50 weight percent builder, between about 50 and weight percent sodium perborate and between about 0.2 and 2 weight percent enzyme.
  • a turbulent air mixer such as that described in British Pat. No. 1,118,908, should conveniently be used for effecting granulation of these components in those cases in which water is the granulating agent, which may be used in combination with further detergent addends, if desired.
  • the solid detergent components which may be premixed, if desired, are fluidized using a stream of air and the liquid detergent components are simultaneously sprayed through nozzles onto the fluidized blend.
  • the air is passed through the turbulent air mixer at a rate and/or temperature sufficient to permit firstly the dissipation of the heat of hydration set free and secondly the maintenance of the temperature which is necessary for the hydration to take a fairly rapid course.
  • the detergent composition produced in accordance with the present invention is a homogeneous granulate composed of homogeneous individual particles that substantially contain the following components:
  • a. builder substances namely alkali metal salts of which the cation is a lithium, sodium, potassium or ammonium ion and the acid salt component is sulfuric acid, silicic acid, disilicic acid, carbonic acid, an oligo or polyphosphoric acid, nitrilotriacetic acid, ethylenediaminetetracetic acid, a homopolymer or copolymer of an unsaturated aliphatic polycarboxylic acid, a copolymer of an unsaturated aliphatic polycarboxylic acid with an alkylene, an unsaturated monocarboxylic acid or further vinyl compound, a copolymer of a vinylphosphonic acid with acrylic acid or a further vinyl compound, a polyvinylphosphonic acid, an aminopolycarboxylic acid, a hydroxyalkylaminopolycarboxylic acid, phytic acid, an alkylenephosphonic acid, a hdyroxyalkylenephosphonic acid or an aminoalkylenephospho
  • binders such as polyvinyl pyrrolidone, cellulose ether, dextrin, alginates, agar-agar, gum arabic, tragacanth, polyvinyl alcohol, bassorin or guar gum, and optionally e. one or more surface-active substances, perfumes, optical brighteners, desinfectants and peroxide stabilizers or activators, such as alkaline earth metal silicates, heavy metal salts or tetracetylethylene diamine.
  • binders such as polyvinyl pyrrolidone, cellulose ether, dextrin, alginates, agar-agar, gum arabic, tragacanth, polyvinyl alcohol, bassorin or guar gum, and optionally e. one or more surface-active substances, perfumes, optical brighteners, desinfectants and peroxide stabilizers or activators, such as alkaline earth metal silicates, heavy metal salts or tetracetylethylene di
  • the builder substances defined under item a) hereinabove comprise more particularly alkali metal salts of which the acid component may be one of the following compounds:
  • the quality of the individual particles forming the granulated detergent composition of the present invention can be improved by dissolving or suspending one of the binders specified above in the spray water.
  • the granulated detergent composition made by the process of the present invention has the distinction of perfectly satisfying the requirements which a modern detergent has to meet, such as good flowability, uniform particle size, constant apparent density and freedom from dust.
  • the perborate has unexpectedly been found not to affect the activity of the enzyme during granulation, and that the perborate remains undecomposed.
  • a further advantage resides in the fact that merely one step is necessary for the production of the detergent composition of the present invention.
  • EXAMPLE 1 A blend of 200 kg sodium tripolyphosphate with a phase-l-content of more than 50 percent and an apparent density of 580 grams/liter,
  • 50 kg lightweight sodium sulfate and 1 kg optical brightener was introduced into a turbulent air mixer and fluidized therein, by means of a stream of air.
  • 50 kg liquid surface-active substance (Genapol 0-120) and 40 kg water having 3.6 kg of a blend of highly active bacterial proteases dissolved therein were sprayed onto the fluidized blend, through separate sets of nozzles arranged in annular fashion.
  • the temperature prevailing in the turbulent air mixer was about 25C.
  • a readily flowable granulated detergent composition was obtained. It had an apparent density of 410 grams/liter and a proteolytic activity of 1,300 Loehlein-Vollhard units, per gram granulated detergent. The sodium perborate could not be found to have been decomposed.
  • EXAMPLE 2 The blend described in Example 1 was prepared and fluidized together with 3.6 kg highly active bacterial protease, in a turbulent air mixer. 40 kg water and 50 kg liquid surfaceactive substance were sprayed onto the fluidized blend, through separate sets of nozzles arranged in annular fashion. The resulting granulate had a proteolytic activity of 1,300 Loehlein-Vollhard units, per gram granulated detergent. The granulate had a good flowability. The perborate remained unchanged.
  • EXAMPLE 3 (Comparative Example) The blend of Example 1 was prepared and fluidized in a turbulent air mixer, by means of a stream of air. 50 kg surface active substance (Genapol O-l 20) and 40 kg water were sprayed onto the fluidized blend, through separate sets of nozzles arranged in annular fashion. The resulting granulated detergent composition was mechanically blended with 3.6 kg of the highly active protease used in Example 1. The finished detergent composition was found to have a proteolytic activity of about 1,300 Leohlein-Vollhard units.
  • EXAMPLE 4 A blend of 290 kg sodium tripolyphosphate with a phase-I-content of more than 50 percent and an apparent density of 590 grams/liter,
  • EXAMPLE 5 A blend of 160 kg sodium tripolyphosphate with a phase-l-content of more than 50 percent and an apparent density of 590 grams/liter,
  • kg powdered soap and 1 kg optical brightener was introduced into a turbulent air mixer and fluidized therein, by means of a stream of air.
  • 90 kg liquid surface active substance (Genapol O-l20) and 120 kg water having 2.0 kg highly active bacterial protease dissolved therein were sprayed onto the fluidized blend, through separate sets of nozzles arranged in annular fashion.
  • the temperature prevailing in the turbulent air mixer was about 22C.
  • a readily flowable granulated detergent composition was obtained. It had an apparent density of 420 grams/liter and a proteolytic activity of 400 Lohlein-Vollhard units, per gram granulated detergent.
  • the builder substance is at least one member selected from the group consisting of sodium tripolyphosphate with a phase-l-content of between 20 and 100 weight percent, sodium pyrophosphate, sodium hexametaphosphate, trisodium nitrilotriacetate and tetrasodium ethylenediaminetetracetate.
  • the detergent composition contains between about 20 and 50 weight percent builder, between about 50 and 10 weight percent sodium perborate and between about 0.2 and 2 weight percent enzyme.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)
US5945A 1969-02-11 1970-01-26 Process for the manufacture of enzyme and perborate-containing detergent compositions Expired - Lifetime US3676352A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19691906705 DE1906705A1 (de) 1969-02-11 1969-02-11 Verfahren zur Herstellung von enzym- und perborathaltigen Vollwaschmitteln
DE19702000069 DE2000069A1 (de) 1969-02-11 1970-01-02 Verfahren zur Herstellung von enzym- und perborathaltigen Vollwaschmitteln
DE2008069 1970-01-02

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US3676352A true US3676352A (en) 1972-07-11

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US5945A Expired - Lifetime US3676352A (en) 1969-02-11 1970-01-26 Process for the manufacture of enzyme and perborate-containing detergent compositions

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US (1) US3676352A (de)
AT (1) AT310330B (de)
BE (1) BE745706A (de)
CH (1) CH541618A (de)
DE (2) DE1906705A1 (de)
FR (1) FR2035318A5 (de)
GB (1) GB1275393A (de)
NL (1) NL7001874A (de)

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4330423A (en) * 1973-06-20 1982-05-18 Henkel Kommanditgesellschaft Auf Aktien Process for the production of solid, pourable washing or cleaning agents with a content of a calcium binding silicate
US4568476A (en) * 1983-08-15 1986-02-04 Lever Brothers Company Enzymatic machine-dishwashing compositions
US4617272A (en) * 1984-04-25 1986-10-14 Economics Laboratory, Inc. Enzyme drying process
US4741851A (en) * 1984-04-02 1988-05-03 Colgate Palmolive Co. Non-caking bleaching detergent composition containing a lower hydrate of sodium perborate
US4767557A (en) * 1985-06-28 1988-08-30 The Procter & Gamble Company Dry bleach and stable enzyme granular composition
US4857223A (en) * 1985-10-03 1989-08-15 Colgate-Palmolive Company Non-caking bleaching detergent composition containing a lower hydrate of sodium perborate
US4863626A (en) * 1985-08-21 1989-09-05 The Clorox Company Encapsulated enzyme in dry bleach composition
US5089167A (en) * 1985-08-21 1992-02-18 The Clorox Company Stable peracid bleaching compositions: organic peracid, magnesium sulfate and controlled amounts of water
US5093021A (en) * 1985-08-21 1992-03-03 The Clorox Company Encapsulated enzyme in dry bleach composition
US5167854A (en) * 1985-08-21 1992-12-01 The Clorox Company Encapsulated enzyme in dry bleach composition
US5254287A (en) * 1985-08-21 1993-10-19 The Clorox Company Encapsulated enzyme in dry bleach composition
US5296161A (en) * 1986-06-09 1994-03-22 The Clorox Company Enzymatic perhydrolysis system and method of use for bleaching
US5364554A (en) * 1986-06-09 1994-11-15 The Clorox Company Proteolytic perhydrolysis system and method of use for bleaching
US5741693A (en) * 1992-07-02 1998-04-21 Novo Nordisk A/S Alkalophilic bacillus SP. AC13 and protease, xylanase, cellulase obtainable therefrom
US20070287650A1 (en) * 2005-12-02 2007-12-13 Garman Company, Inc. Powdered Evaporator Coil Cleaner
US20090156454A1 (en) * 2006-04-20 2009-06-18 Henkel Ag & Co. Kgaa Granulates for a sensitive washing- or cleaning agent containing material
US20140287485A1 (en) * 2010-10-15 2014-09-25 Institut National De La Recherche Agronomique Product and method for the removal of biofilms

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1334389C (en) * 1986-03-26 1995-02-14 Ernest H. Brumbaugh Machine dishwasher water spot control composition

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3451935A (en) * 1966-04-25 1969-06-24 Procter & Gamble Granular enzyme-containing laundry composition
US3519570A (en) * 1966-04-25 1970-07-07 Procter & Gamble Enzyme - containing detergent compositions and a process for conglutination of enzymes and detergent compositions
US3538004A (en) * 1966-03-09 1970-11-03 Knapsack Ag Process for the manufacture of detergent compositions

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3538004A (en) * 1966-03-09 1970-11-03 Knapsack Ag Process for the manufacture of detergent compositions
US3451935A (en) * 1966-04-25 1969-06-24 Procter & Gamble Granular enzyme-containing laundry composition
US3519570A (en) * 1966-04-25 1970-07-07 Procter & Gamble Enzyme - containing detergent compositions and a process for conglutination of enzymes and detergent compositions

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4330423A (en) * 1973-06-20 1982-05-18 Henkel Kommanditgesellschaft Auf Aktien Process for the production of solid, pourable washing or cleaning agents with a content of a calcium binding silicate
US4755319A (en) * 1973-06-20 1988-07-05 Henkel Kommanditgellschaft Auf Aktien Process for the production of solid, pourable washing or cleaning agents with a content of a calcium binding silicate
US4568476A (en) * 1983-08-15 1986-02-04 Lever Brothers Company Enzymatic machine-dishwashing compositions
US4741851A (en) * 1984-04-02 1988-05-03 Colgate Palmolive Co. Non-caking bleaching detergent composition containing a lower hydrate of sodium perborate
US4617272A (en) * 1984-04-25 1986-10-14 Economics Laboratory, Inc. Enzyme drying process
US4767557A (en) * 1985-06-28 1988-08-30 The Procter & Gamble Company Dry bleach and stable enzyme granular composition
US5167854A (en) * 1985-08-21 1992-12-01 The Clorox Company Encapsulated enzyme in dry bleach composition
US4863626A (en) * 1985-08-21 1989-09-05 The Clorox Company Encapsulated enzyme in dry bleach composition
US5089167A (en) * 1985-08-21 1992-02-18 The Clorox Company Stable peracid bleaching compositions: organic peracid, magnesium sulfate and controlled amounts of water
US5093021A (en) * 1985-08-21 1992-03-03 The Clorox Company Encapsulated enzyme in dry bleach composition
US5254287A (en) * 1985-08-21 1993-10-19 The Clorox Company Encapsulated enzyme in dry bleach composition
US4857223A (en) * 1985-10-03 1989-08-15 Colgate-Palmolive Company Non-caking bleaching detergent composition containing a lower hydrate of sodium perborate
US5364554A (en) * 1986-06-09 1994-11-15 The Clorox Company Proteolytic perhydrolysis system and method of use for bleaching
US5296161A (en) * 1986-06-09 1994-03-22 The Clorox Company Enzymatic perhydrolysis system and method of use for bleaching
US5741693A (en) * 1992-07-02 1998-04-21 Novo Nordisk A/S Alkalophilic bacillus SP. AC13 and protease, xylanase, cellulase obtainable therefrom
US20070287650A1 (en) * 2005-12-02 2007-12-13 Garman Company, Inc. Powdered Evaporator Coil Cleaner
US7338564B2 (en) * 2005-12-02 2008-03-04 Garman Company, Inc. Powdered evaporator coil cleaner
US20090156454A1 (en) * 2006-04-20 2009-06-18 Henkel Ag & Co. Kgaa Granulates for a sensitive washing- or cleaning agent containing material
US20140287485A1 (en) * 2010-10-15 2014-09-25 Institut National De La Recherche Agronomique Product and method for the removal of biofilms
US11365374B2 (en) 2010-10-15 2022-06-21 S.A. Realco Product and method for removal of biofilms

Also Published As

Publication number Publication date
AT310330B (de) 1973-09-25
GB1275393A (en) 1972-05-24
NL7001874A (de) 1970-08-13
BE745706A (fr) 1970-08-08
DE1906705A1 (de) 1970-08-13
DE2000069A1 (de) 1971-07-08
CH541618A (de) 1973-10-31
FR2035318A5 (de) 1970-12-18

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