US3917741A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method of making polyurethane powder
Assignee: DVSG Holding GmbH
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Filing: 1973-05-09
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Granted: 1975-11-04
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Expires: 1993-05-09
Abstract
Abstract Method for preparing polyurethane resin directly in finely divided form in which method a first reactant for forming the polyurethane is emulsified as fine droplets with the aid of special surfactants and controls in an inert organic liquid medium in which it and polyurethane resin are insoluble, a second reactant for combination with the first reactant is introduced into the liquid medium and interacted interfacially with the droplets of the first reactant to form fine particles of solid polyurethane resin protected from agglomeration by the surfactant, and the particles of polyurethane resin are separated from the liquid medium.
Inventors
- 👤 John J Mcgarr
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 02:30
CPC Classifications
C; C08; C08G; C08G18/00; C08G18/06; C08G18/08; C08G18/10; Y; Y10; Y10S; Y10S528/00; Y10S528/902; Y10S528/906
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
500 words
THE METHOD FOR PREPARING POLYURETHANE RESINS DIRECTLY IN FINELY DIVIDED FORM FROM REACTION OF A FRIST REACTANT COMPRISING AT LEAST ONE ORGANIC POLYISOCYANATE WITH A SECOND REACTANT COMPRISING AT LEAST ONE ORGANIC COMPOUND CONTAINING AT LEAST TWO GROUPS HAVING ACTIVE HYDROGEN TO FORM A SOLID REACTION PRODUCT, SAID FRIST REACTANT BEING EMPLOYED IN AMOUNT RELATIVE TO THE AMOUNT OF SAID SECOND REACTANT TO GIVE A MOLAR RATIO OF ACTIVE HYDROGEN TO -NCO IN THE RANGE OF FROM ABOUT 0.85:1 TO ABOUT 1.15:1, SAID METHOD COMPRISING THE STEPS OF EMULSIFYING, SAID ACTIVE HYDROGEN COMPOUND REACTANT IN LIQUID FORM WITH THE AID OF A POLYMERIC SURFACTANT AS FINE DROPLETS IN A CONTINUOUS PHASE COMPRISING AN ORGANIC LIQUID INERT TO AND LESS POLAR THAN SAID REACTANT AND IN WHICH AT LEAST SAID ONE REACTANT AND SAID SOLID REACTION PRODUCT ARE SUBSTANTIALLY INSOLUBLE AND THE OTHER OF SAID REACTANTS IS MISCIBLE, SAID SUFACTANT BEING PRESENT IN AMOUNT OF FROM ABOUT 0.1% TO ABOUT 10% ON THE WEIGHT OF EMULSIFIED INSOLUBLE LIQUID REACTANT, DISSOLVING SAID MISCIBLE REACTANT IN SAID INERT ORGANIC LIQUID, REACTING SAID EMULSIFIED INSOLUBLE REACTANTS WITH SAID MISCIBLE DISSOLVED REACTANT BY INTERFACIAL REACTION BETWEEN THE DROPLETS OF SAID EMULSIFIED REACTANT AND DISSOLVED REACTANT IN SAID INERT ORGANIC LIQUID UNDER CONDITIONS OF VIGOROUS AGITATION TO FORM TFINE PARTICLES OF SAID POLYURETHANE SEPARABLE FROM SAID INERT LIQUID BY SETTLING, AND SEPARATING SAID PARTICLES FROM SAID INERT LIQUID, THE MOLECULES OF SAID POLYMERIC SUFACTANT HAVING AN AVERAGE MOLECULAR WEIGHT OF AT LEAST ABOUT 2,000, AND HAVING POLAR GROUPS WHICH ASSOCIATE WITH THE SURFACE OF SAID DROPLETS OF EMULSIFIED INSOLUBLE REACTANT AND WITH PARTICLES OF SAID SOLID REACTION PRODUCT AND LESS-POLAR GROUPS WHICH ARE SOLVATED BY THE SAID INERT ORGANIC LIQUID, THE QUANTITY AND THE BALANCE OF POLAR TO LESS-POLAR GROUPS OF SAID SURFACTANT RELATIVE TO THE POLARITIES OF SAID INERT ORGANIC LIQUID, SAID INSOLUBLE EMULSIFIED LIQUID REACTANT AND SAID REACTION PRODUCT PROVIDING THAT THE TOTAL ASSOCIATION OF LESS POLAR GROUPS WITH SAID INERT ORGANIC LIQUID IS GREATER THAN THE TOTAL ASSOCIATION OF THE POLAR GROUPS WITH SAID EMULSIFIED INSOLUBLE REACTANT AND WITH SAID SOLID REACTION PRODUCT BY AN AMOUNT TO ENSURE THAT SAID INERT LIQUID WILL BE THE EXTERNAL PHASE, BUT IS LESS THAN THE AMOUNT WHICH WOULD INTERFERE WITH FORMATION OF A FINE EMULSION OF THE INSOLUBLE LIQUID REACTANT IN SAID ORGANIC LIQUID, COORINATING (A) THE INTENSITY OF SAID AGITATION, (B) THE QUANTITY AND THE BALANCE OF POLAR TO LESS-POLAR GROUPS OF SAID SUFACTANT IN SAID EMULSION AND (C) THE POLARITIES OF SAID INERT ORGANIC LIQUID, SAID EMULSIFIED INSOLUBLE LIQUID REACTANT AND SAID REACTION PRODUCT TO FORM A FINE EMULSION IN WHICH AT LEAST ABOUT 95% BY WEIGHT OF THE DROPLETS OF SAID EMULSIFIED REACTANT WILL BE IN THE RANGE OF FROM 1 TO 300 MICRONS IN DIAMETER SO THAT THE PARTICLES OF REACTION PRODUCT WILL SETTLE, THE ASSOCIATION O F SAID SURFACTANT WITH SAID REACTION PRODUCT HOLDING SAID SURFACTANT ON THE SURFACE OF SAID PARTICLES OF REACTION PRODUCT TO IMPEDE AGGLOMERATION OF SAID PARTICLES.
Claim 2
Independent Claim
500 words
THE METHOD FOR PREPARING POLYURETHANE RESINS DIRECTLY IN FINELY DIVIDED FORM FROM REACTION OF A FRIST REACTANT COMPRISING AT LEAST ONE ORGANIC POLYISOCYANATE WITH A SECOND REACTANT COMPRISING AT LEAST ONE ORGANIC COMPOUND CONTAINING AT LEAST TWO GROUPS HAVING ACTIVE HYDROGEN TO FORM A SOLID REACTION PRODUCT, SAID FRIST REACTANT BEING EMPLOYED IN AMOUNT RELATIVE TO THE AMOUNT OF SAID SECOND REACTANT TO GIVE A MOLAR RATIO OF ACTIVE HYDROGEN TO -NCO IN THE RANGE OF FROM ABOUT 0.85:1 TO ABOUT 1.15:1, SAID METHOD COMPRISING THE STEPS OF EMULSIFYING, SAID ACTIVE HYDROGEN COMPOUND REACTANT IN LIQUID FORM WITH THE AID OF A POLYMERIC SURFACTANT AS FINE DROPLETS IN A CONTINUOUS PHASE COMPRISING AN ORGANIC LIQUID INERT TO AND LESS POLAR THAN SAID REACTANT AND IN WHICH AT LEAST SAID ONE REACTANT AND SAID SOLID REACTION PRODUCT ARE SUBSTANTIALLY INSOLUBLE AND THE OTHER OF SAID REACTANTS IS MISCIBLE, SAID SUFACTANT BEING PRESENT IN AMOUNT OF FROM ABOUT 0.1% TO ABOUT 10% ON THE WEIGHT OF EMULSIFIED INSOLUBLE LIQUID REACTANT, DISSOLVING SAID MISCIBLE REACTANT IN SAID INERT ORGANIC LIQUID, REACTING SAID EMULSIFIED INSOLUBLE REACTANTS WITH SAID MISCIBLE DISSOLVED REACTANT BY INTERFACIAL REACTION BETWEEN THE DROPLETS OF SAID EMULSIFIED REACTANT AND DISSOLVED REACTANT IN SAID INERT ORGANIC LIQUID UNDER CONDITIONS OF VIGOROUS AGITATION TO FORM TFINE PARTICLES OF SAID POLYURETHANE SEPARABLE FROM SAID INERT LIQUID BY SETTLING, AND SEPARATING SAID PARTICLES FROM SAID INERT LIQUID, THE MOLECULES OF SAID POLYMERIC SUFACTANT HAVING AN AVERAGE MOLECULAR WEIGHT OF AT LEAST ABOUT 2,000, AND HAVING POLAR GROUPS WHICH ASSOCIATE WITH THE SURFACE OF SAID DROPLETS OF EMULSIFIED INSOLUBLE REACTANT AND WITH PARTICLES OF SAID SOLID REACTION PRODUCT AND LESS-POLAR GROUPS WHICH ARE SOLVATED BY THE SAID INERT ORGANIC LIQUID, THE QUANTITY AND THE BALANCE OF POLAR TO LESS-POLAR GROUPS OF SAID SURFACTANT RELATIVE TO THE POLARITIES OF SAID INERT ORGANIC LIQUID, SAID INSOLUBLE EMULSIFIED LIQUID REACTANT AND SAID REACTION PRODUCT PROVIDING THAT THE TOTAL ASSOCIATION OF LESS POLAR GROUPS WITH SAID INERT ORGANIC LIQUID IS GREATER THAN THE TOTAL ASSOCIATION OF THE POLAR GROUPS WITH SAID EMULSIFIED INSOLUBLE REACTANT AND WITH SAID SOLID REACTION PRODUCT BY AN AMOUNT TO ENSURE THAT SAID INERT LIQUID WILL BE THE EXTERNAL PHASE, BUT IS LESS THAN THE AMOUNT WHICH WOULD INTERFERE WITH FORMATION OF A FINE EMULSION OF THE INSOLUBLE LIQUID REACTANT IN SAID ORGANIC LIQUID, COORINATING (A) THE INTENSITY OF SAID AGITATION, (B) THE QUANTITY AND THE BALANCE OF POLAR TO LESS-POLAR GROUPS OF SAID SUFACTANT IN SAID EMULSION AND (C) THE POLARITIES OF SAID INERT ORGANIC LIQUID, SAID EMULSIFIED INSOLUBLE LIQUID REACTANT AND SAID REACTION PRODUCT TO FORM A FINE EMULSION IN WHICH AT LEAST ABOUT 95% BY WEIGHT OF THE DROPLETS OF SAID EMULSIFIED REACTANT WILL BE IN THE RANGE OF FROM 1 TO 300 MICRONS IN DIAMETER SO THAT THE PARTICLES OF REACTION PRODUCT WILL SETTLE, THE ASSOCIATION O F SAID SURFACTANT WITH SAID REACTION PRODUCT HOLDING SAID SURFACTANT ON THE SURFACE OF SAID PARTICLES OF REACTION PRODUCT TO IMPEDE AGGLOMERATION OF SAID PARTICLES.
Claim 3
Dependent Claim
71 words
The method for preparing polyurethane resins directly in finely divided form as defined in claim 1 in which said emulsified insoluble reactant in said compound containing groups having active hydrogen and said surfactant is a copolymer of two types of monomer of which one, if homopolymerized, would have a polarity compatible with the emulsified reactant and the other, if homopolymerized, would have a lower polarity compatible with the inert organic liquid.
Claim 4
Dependent Claim
76 words
The method for preparing polyurethane resins directly in finely divided form as defined in claim 2 in which the intensity of agitation, the quantity and balance of polar to less-polar groups of said surfactant and the polarities of said insoluble reactant and said reaction product are coordinated to provide that at least about 95% by weight of the particles of reaction product are in the range of from about 5 to about 75 microns in diameter.
Claim 5
Dependent Claim
139 words
The method for preparing polyurethane resins directly in finely divided form as defined in claim 3 in which the ratio of active hydrogens to -NCO of said reactants is in the range of from about 0.95:1 to about 1.05:1, in which said reactants constitute up to about 60% by weight of the total weight of reaction mixture and the inert organic liquid is an aliphatic hydrocarbon liquid having a boiling point in the range of from about 65*C. to about 200*C. and in which said surfactant is a copolymer of at least one acrylic or methacrylic acid ester of an alcohol having at least four carbon atoms to provide the less-polar groups and at least one acrylic or methacrylic acid ester of a member of the group consisting of methyl alcohol, and N,N-diethylaminoethyl alcohol to provide the polar groups.
Claim 6
Dependent Claim
52 words
The method for preparing polyurethane resins directly in finely divided form as defined in claim 4 in which said surfactant is the product of grafting methylmethacrylate monomer to polylaurylmethaorylate in proportion to give a mole ratio of methyl to lauryl groups of 1:1.7, the product having a molecular weight of about 22,000.
Claim 7
Dependent Claim
49 words
The method for preparing polyurethane resins directly in finely divided form as defined in claim 4 in which said surfactant is a block copolymer of polylaurylmethacrylate and polymethylmethacrylate in which the mole ratio of methyl groups to lauryl groups is about 1.1:1 and the molecular weight is about 8,400.
Claim 8
Dependent Claim
48 words
The method for preparing polyurethane resins directly in finely divided form as divided in claim 4 in which said surfactant is a linear copolymer of laurylmethacrylate and N,N-diethylaminoethylmethacrylate in which the mole ratio of lauryl groups to diethylaminoethyl groups is 1.2:1 and the molecular weight is about 3,700.
Claim 9
Dependent Claim
44 words
The method for preparing polyurethane resins directly in finely divided form as defined in claim 2 in which said emulsified insoluble reactant comprises at least one -OH terminated polyester or polyalkylene ether polyol having a molecular weight of from about 300 to about 4,000.
Claim 10
Dependent Claim
33 words
The method for preparing polyurethane resins directly in finely divided form as defined in claim 8 in which said soluble reactant is a member of the group consisting of aromatic and cycloaliphatic diisocyanates.
Claim 11
Dependent Claim
36 words
The method for preparing polyurethane resins directly in finely divided form as defined in claim 9 in which said diisocyanate is added to an already formed emulsion of said insoluble reactant under conditions of vigorous agitation.
References Cited (Backward Citations)
US3317635A
Cited
US3236812A
Cited
US3382297A
Cited
US3405087A
Cited
US3472798A
Cited
US3428711A
Cited
US3716505A
Cited
US3763065A
Cited
US3773857A
Cited
US3787525A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-11-03 | 1979-05-05 | 1979-11-04 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-11-03 | 1983-05-05 | 1983-11-04 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-11-03 | 1987-05-05 | 1987-11-04 | $7700.00 | Window Closed / Lapsed |