US3737376A - Non-dusting and moisture-resistant enzyme compositions - Google Patents

Non-dusting and moisture-resistant enzyme compositions Download PDF

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Publication number
US3737376A
US3737376A US00061416A US3737376DA US3737376A US 3737376 A US3737376 A US 3737376A US 00061416 A US00061416 A US 00061416A US 3737376D A US3737376D A US 3737376DA US 3737376 A US3737376 A US 3737376A
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Prior art keywords
enzyme
dusting
bacterial
petrolatum
moisture
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US00061416A
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J Ziffer
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PMP ACQUISITION Corp A DE CORP
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Pabst Brewing Co
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Assigned to FIRST WISCONSIN NATIONAL BANK OF MILWAUKEE, A NATIONAL BANKING ASSOCIATION, AS AGENT reassignment FIRST WISCONSIN NATIONAL BANK OF MILWAUKEE, A NATIONAL BANKING ASSOCIATION, AS AGENT SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: PABST BREWING COMPANY A DE CORP.
Assigned to PMP ACQUISITION CORPORATION, A DE CORP. reassignment PMP ACQUISITION CORPORATION, A DE CORP. ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: PAPST BREWING COMPANY
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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/38Products with no well-defined composition, e.g. natural products
    • C11D3/386Preparations containing enzymes, e.g. protease or amylase
    • C11D3/38672Granulated or coated enzymes

Definitions

  • One of the ojects of the present invention is to provide dry-appearing, essentially non-dusting, flowable enzyme powders free of gummy, sticky and lumpy characteristics comprising a finely divided solid enzyme of the type used in the preparation of pre-soak and detergent washing products, namely, bacterial protease, bacterial amylase and mixtures of bacterial protease and bacterial amylase.
  • a further object of the invention is to provide new and improved flowable enzyme powders of the type described by the use of readily available, inexpensive, non-toxic modifying ingredients.
  • Another object of the invention is to provide a new and improved process for producing dry-appearing, essentially non-dusting, flowable enzyme powders of the type described. Other objects will appear hereinafter.
  • a dry-appearing, essentially non-dusting, flowable enzyme powder free of gummy, sticky, and lumpy characteristics comprising a finely divided solid enzyme from the group consisting of bacterial protease, bacterial amylase and mixtures of bacterial protease and bacterial amylase with or without other ingredients, as, for example, calcium acetate monohydrate, sodium sulfite, sodium sulfate, sodium tripolyphosphate, calcium carbonate and monocalcium phosphate, is prepared by intimately mixing with said enzyme with or without said other ingredients a dust and moisture inhibiting substance in the form of petrolatum or petrolatum liquid, or mixtures of petrolatum and petrolatum liquid, in an amount suflicient to reduce the dusting characteristic and impart protection against moisture but insuflicient to produce gummy, sticky and lumpy characteristics and interfere with flowability.
  • a dust and moisture inhibiting substance in the form of petrolatum or petrolatum liquid, or mixtures of petrolatum and petrolatum liquid, in an amount
  • petrolatum and petrolatum liquid as used herein are defined in the Merck Index, 8th edition, page 800.
  • a preferred type of petrolatum liquid is a mineral oil having a Sayboldt viscosity of 65/75 at F. (37.8 C.). The same product is available in a range of Saybolt viscosity of 48/52 to /155, as well as a viscosity of 180/190. Hence, a general range of viscosity is from 48 to 190.
  • the petrolatum is a yellowish to light amber or white, semi-solid, unctuous jelly. Either or both of these types of substances and mixtures thereof are effective for the purpose of the invention.
  • the amounts required are normally within the range of 1% to 10% of the weight of the enzymes and a preferred range is 3% to 8% by weight of the enzymes.
  • the protease of the enzymes is defined in terms of PV units per gram for bacterial protease and DV units per gram for bacterial amylase.
  • the PV activity of the bacterial protease will usually be within the range of 15,000 to 1,000,000 PV units per gram and the potency of the bacterial amylase will usually be within the range of 30 to 100,000 DV units per gram. In some enzyme compositions the amount of bacterial amylase is not significant.
  • the dust and moisture inhibiting petrolatum and petrolatum liquid or mixtures thereof can be used to prepare non-dusting, flowable enzyme powders consisting essentially of the enzymes per se. They can also be used to prepare enzyme compositions which are essentially dryappearing, non-dusting and flowable and contain diluents such as, for example, calcium acetate monohydrate, sodium sulfite, sodium sulfate, sodium tripolyphosphate, calcium carbonate and monocalcium phosphate. In some cases other substances can be added for special purposes.
  • the mixture was ground during and after the addition of the petrolatum and/or petrolatum liquid to a desired particle size, for example, a size sufficient to pass a 325 mesh sieve.
  • teristics consisting essentially of a finely divided solid enzyme from the group consisting of bacterial protease, bacterial amylase and mixtures of bacterial protease and bacterial amylase, intimately mixed with a dust and moisture inhibiting substance from the group consisting of petrolatum, petrolatum liquid and mixtures thereof in an amount sufiicient to reduce the dusting characteristic and impart protection against moisture but insufiicient to produce gummy, sticky and lumpy characteristics and interfere with flowability.
  • composition as claimed in claim 1 in which said dust and moisture inhibiting substance is petrolatum.
  • a composition as claimed in claim 1 in which said dust and moisture inhibiting substance is petrolatum liquid.
  • composition as claimed in claim 1 in which the percentage of said dust and moisture inhibiting substance is 1% to of the weight of said enzyme.
  • composition as claimed in claim 1 in which the percentage of said dust and moisture inhibiting substance is 3% to 8% of the weight of said enzyme.
  • composition as claimed in claim 1 in which said petrolatum is a mineral oil having a Saybolt viscosity within the range of 48 to 190 at 100 F.
  • composition as claimed in claim 1 in which said enzyme comprises a bacterial protease having a PV activity within the range of 15,000 to 1,000,000 PV units per gram.
  • composition as claimed in claim 1 in which said enzyme is a mixture of bacterial protease and bacterial amylase, the activity of said mixture being within the 100,000 DV units per gram.
  • An enzyme composition as claimed in claim 1 consisting essentially of an enzyme from the group consisting of bacterial protease, bacterial amylase and mixtures of bacterial protease and bacterial amylase intimately mixed with 3% to 8% mineral oil.
  • a process of preparing a dry-appearing, essentially non-dusting, flowable enzyme powder free of gummy, sticky and lumpy characteristics which consists essentially of intimately mixing a finely divided solid enzyme from the group consisting of bacterial protease, bacterial amylase and mixtures of bacterial protease and bacterial amylase with a dust and moisture inhibiting substance from the group consisting of petrolatum, petrolatum liquid, and mixtures thereof in an amount sufficient to reduce the dusting characteristic of the resultant product in its powder state and impart protection against moisture but insuflicient to interfere with flowability of said powder product.

Abstract

ENZYME COMPOSITIONS OF THE TYPE USED IN WASHING NAMELY, BACTERIAL PROTEASE, BACTERIAL AMYLASE AND MIXTURES THEREOF ARE PREPARED IN THE FORM OF A DRY-APPEARING, ESSENTIALLY NON-DUSTING, FLOWABLE ENZYME POWDER, FREE OF GUMMY, STICKY AND LUMPY CHARACTERISTICS AND RESISTANT TO MOISTURE.

Description

United States Patent O 3,737,376 NON-DUSTING AND MOISTURE-RESISTANT ENZYME COMPOSITIONS Jack Zifier, Milwaukee, Wis., assignor to Pabst Brewing Company, Milwaukee, Wis. No Drawing. Filed Aug. 5, 1970, Ser. No. 61,416
Int. Cl. ClZk 1/00 US. Cl. 195-63 11 Claims ABSTRACT OF THE DISCLOSURE Enzyme compositions of the type used in washing, namely, bacterial protease, bacterial amylase and mixtures thereof are prepared in the form of a dry-appearing, essentially non-dusting, flowable enzyme powder, free of gummy, sticky and lumpy characteristics and resistant to moisture.
BACKGROUND OF THE INVENTION In recent years the use of enzymes, especially bacterial protease for pre-soak and detergent washing products has greatly increased. These enzymes are now being produced in very high potency concentrations and handling problems have developed as a result of these high potency levels. Many individuals have found these enzymes to be a source of irritation. The problem is particularly acute in the manufacture and handling of the enzymes themselves and also in the handling of the enzymes in plants where they are formulated into various types of detergent products. The problem would be greatly alleviated if it were possible to produce a dust-free enzyme product.
OBJECTS One of the ojects of the present invention is to provide dry-appearing, essentially non-dusting, flowable enzyme powders free of gummy, sticky and lumpy characteristics comprising a finely divided solid enzyme of the type used in the preparation of pre-soak and detergent washing products, namely, bacterial protease, bacterial amylase and mixtures of bacterial protease and bacterial amylase.
A further object of the invention is to provide new and improved flowable enzyme powders of the type described by the use of readily available, inexpensive, non-toxic modifying ingredients.
Another object of the invention is to provide a new and improved process for producing dry-appearing, essentially non-dusting, flowable enzyme powders of the type described. Other objects will appear hereinafter.
GENERAL STATEMENT OF THE INVENTION In accordance with the invention a dry-appearing, essentially non-dusting, flowable enzyme powder free of gummy, sticky, and lumpy characteristics comprising a finely divided solid enzyme from the group consisting of bacterial protease, bacterial amylase and mixtures of bacterial protease and bacterial amylase with or without other ingredients, as, for example, calcium acetate monohydrate, sodium sulfite, sodium sulfate, sodium tripolyphosphate, calcium carbonate and monocalcium phosphate, is prepared by intimately mixing with said enzyme with or without said other ingredients a dust and moisture inhibiting substance in the form of petrolatum or petrolatum liquid, or mixtures of petrolatum and petrolatum liquid, in an amount suflicient to reduce the dusting characteristic and impart protection against moisture but insuflicient to produce gummy, sticky and lumpy characteristics and interfere with flowability.
Patented June 5, 1973 The terms petrolatum and petrolatum liquid as used herein are defined in the Merck Index, 8th edition, page 800. A preferred type of petrolatum liquid is a mineral oil having a Sayboldt viscosity of 65/75 at F. (37.8 C.). The same product is available in a range of Saybolt viscosity of 48/52 to /155, as well as a viscosity of 180/190. Hence, a general range of viscosity is from 48 to 190. The petrolatum is a yellowish to light amber or white, semi-solid, unctuous jelly. Either or both of these types of substances and mixtures thereof are effective for the purpose of the invention. The amounts required are normally within the range of 1% to 10% of the weight of the enzymes and a preferred range is 3% to 8% by weight of the enzymes.
The protease of the enzymes is defined in terms of PV units per gram for bacterial protease and DV units per gram for bacterial amylase. The PV activity of the bacterial protease will usually be within the range of 15,000 to 1,000,000 PV units per gram and the potency of the bacterial amylase will usually be within the range of 30 to 100,000 DV units per gram. In some enzyme compositions the amount of bacterial amylase is not significant.
The dust and moisture inhibiting petrolatum and petrolatum liquid or mixtures thereof can be used to prepare non-dusting, flowable enzyme powders consisting essentially of the enzymes per se. They can also be used to prepare enzyme compositions which are essentially dryappearing, non-dusting and flowable and contain diluents such as, for example, calcium acetate monohydrate, sodium sulfite, sodium sulfate, sodium tripolyphosphate, calcium carbonate and monocalcium phosphate. In some cases other substances can be added for special purposes.
DETAILED DESCRIPTION OF THE INVENTION In preparing compositions in accordance with the invention several different methods were used as follows:
(A) Mineral oil was blended at ordinary temperatures and pressures either as such or as a fine spray with the finely divided enzyme either alone or mixed with other ingredients;
(B) Mineral oil was blended with a mixture of the enzyme and other ingredients, except sodium sulfate and sodium sulfate was intimately mixed with the resultant product after the mineral oil addition;
(C) Mineral oil was blended vw'th the enzyme and other ingredients except calcium acetate and sodium sulfate and calcium acetate and sodium sulfate were intimately mixed with the resultant composition after the mineral oil addition; and
(D) The enzyme with or without other ingredients was prewarmed to a temperature of about 50 C. and then slowly intimately mixed vw'th a warm solution of petrolatum or a mixture of petrolatum and petrolatum liquid which had been previously warmed to about 50 C. After all of the petrolatum or petrolatum liquid had been added, blending Was continued until the mixture was uniform while allowing it to cool.
In some cases the mixture was ground during and after the addition of the petrolatum and/or petrolatum liquid to a desired particle size, for example, a size sufficient to pass a 325 mesh sieve.
In the following tables in which the quantities are given in parts by weight unless otherwise indicated, calcium acetate monohydrate is symbolized by Ca(OAc) sodium tripolyphosphate by STP, sodium sulfite by Na SO zinc oxide by ZnO, sodium sulfate by Na SO calcium carbonate by CaCO and monocalcium phosphate by MCP. The method of addition is given in the last column of each table.
teristics consisting essentially of a finely divided solid enzyme from the group consisting of bacterial protease, bacterial amylase and mixtures of bacterial protease and bacterial amylase, intimately mixed with a dust and moisture inhibiting substance from the group consisting of petrolatum, petrolatum liquid and mixtures thereof in an amount sufiicient to reduce the dusting characteristic and impart protection against moisture but insufiicient to produce gummy, sticky and lumpy characteristics and interfere with flowability.
2. A composition as claimed in claim 1 in which said dust and moisture inhibiting substance is petrolatum.
3. A composition as claimed in claim 1 in which said dust and moisture inhibiting substance is petrolatum liquid.
4. A composition as claimed in claim 1 in which the percentage of said dust and moisture inhibiting substance is 1% to of the weight of said enzyme.
5. A composition as claimed in claim 1 in which the percentage of said dust and moisture inhibiting substance is 3% to 8% of the weight of said enzyme.
6. A composition as claimed in claim 1 in which said petrolatum is a mineral oil having a Saybolt viscosity within the range of 48 to 190 at 100 F.
7. A composition as claimed in claim 1 in which said enzyme comprises a bacterial protease having a PV activity within the range of 15,000 to 1,000,000 PV units per gram.
8. A composition as claimed in claim 1 in which said enzyme comprises bacterial amylase having an activity of 30 to 100,000 DV units per gram.
9. A composition as claimed in claim 1 in which said enzyme is a mixture of bacterial protease and bacterial amylase, the activity of said mixture being within the 100,000 DV units per gram.
10. An enzyme composition as claimed in claim 1 consisting essentially of an enzyme from the group consisting of bacterial protease, bacterial amylase and mixtures of bacterial protease and bacterial amylase intimately mixed with 3% to 8% mineral oil.
11. A process of preparing a dry-appearing, essentially non-dusting, flowable enzyme powder free of gummy, sticky and lumpy characteristics which consists essentially of intimately mixing a finely divided solid enzyme from the group consisting of bacterial protease, bacterial amylase and mixtures of bacterial protease and bacterial amylase with a dust and moisture inhibiting substance from the group consisting of petrolatum, petrolatum liquid, and mixtures thereof in an amount sufficient to reduce the dusting characteristic of the resultant product in its powder state and impart protection against moisture but insuflicient to interfere with flowability of said powder product.
References Cited UNITED STATES PATENTS 2,642,376 6/1953 Gale et al. 195-63 2,958,632 11/1960 Schwarz et al. 195-68 3,164,523 1/1965 Fox et al. 19563 3,519,570 7/1970 McCarty 252Digest 3,560,392 2/1971 Eymerg et al. 252Digest OTHER REFERENCES Rose, The Cond. Chem. Dict., 7th ed., 1966, Reinhold Publ. Co., pp. 723-724.
WILLIAM E. SCHULZ, Primary Examiner US. Cl. X.R.
mg UNITED STATES PATENT oFFicE CEFRTFFICATE OF CURRECTEGN PatentNo- 5,757,576 Dated June 5, 1975 Inventofls) Jack Ziff'er' It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:
Column 5, Table I, Example 9, "45,940" should read +1340 Column A, Table 11', Example 29, under "STP"; insert O Signed and sealed this 25th day of December 1973.
(SEAL) Attest:
EDWARD M. FLETCHER,JR. RENE D. TEGTMEYER Attesting Officer Acting Commissioner of Patents
US00061416A 1970-08-05 1970-08-05 Non-dusting and moisture-resistant enzyme compositions Expired - Lifetime US3737376A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996000773A1 (en) * 1994-06-28 1996-01-11 Henkel Kommanditgesellschaft Auf Aktien Production of multiple enzyme granulates
WO1996016151A1 (en) * 1994-11-18 1996-05-30 Genencor International, Inc. Coated enzyme granules
WO2002020746A1 (en) 2000-09-08 2002-03-14 Novozymes A/S Lubricated granules
US20020119201A1 (en) * 2000-09-08 2002-08-29 Novozymes A/S Lubricated granules
JP2009529324A (en) * 2006-03-10 2009-08-20 ビーエーエスエフ ソシエタス・ヨーロピア Solid phase enzyme preparation and method for producing the same

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996000773A1 (en) * 1994-06-28 1996-01-11 Henkel Kommanditgesellschaft Auf Aktien Production of multiple enzyme granulates
US5972668A (en) * 1994-06-28 1999-10-26 Henkel Kommanditgesellschaft Auf Aktien Production of multi-enzyme granules
WO1996016151A1 (en) * 1994-11-18 1996-05-30 Genencor International, Inc. Coated enzyme granules
WO2002020746A1 (en) 2000-09-08 2002-03-14 Novozymes A/S Lubricated granules
US20020119201A1 (en) * 2000-09-08 2002-08-29 Novozymes A/S Lubricated granules
EP1317533A1 (en) * 2000-09-08 2003-06-11 Novozymes A/S Lubricated granules
JP2004508040A (en) * 2000-09-08 2004-03-18 ノボザイムス アクティーゼルスカブ Lubricated granules
JP2009529324A (en) * 2006-03-10 2009-08-20 ビーエーエスエフ ソシエタス・ヨーロピア Solid phase enzyme preparation and method for producing the same
JP2012161326A (en) * 2006-03-10 2012-08-30 Basf Se Solid enzyme formulations and process for their preparation
JP2015165809A (en) * 2006-03-10 2015-09-24 ビーエーエスエフ ソシエタス・ヨーロピアBasf Se Solid enzyme formulations and process for their preparation

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Owner name: LAWYERS TITLE COMPANY OF WASHINGTON, INC. (TRUSTEE

Free format text: SECURITY INTEREST;ASSIGNOR:PABST BREWING COMPANY A DE CORP.;REEL/FRAME:004129/0649

Effective date: 19830321

Owner name: FIRST WISCONSIN NATIONAL BANK OF MILWAUKEE, A NATI

Free format text: SECURITY INTEREST;ASSIGNOR:PABST BREWING COMPANY A DE CORP.;REEL/FRAME:004129/0649

Effective date: 19830321

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Owner name: PMP ACQUISITION CORPORATION, A DE CORP.

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:PAPST BREWING COMPANY;REEL/FRAME:004390/0892

Effective date: 19841231