Patent US3923742A successfully refreshed from Google Patents.
US3923742A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for the production of polycarboxylates having improved biological degradability
Assignee: Individual
•
Filing: 1974-11-11
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Granted: 1975-12-02
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Expires: 1994-11-11
Abstract
Abstract A process for the production of a polycarboxylate comprising oxidatively polymerizing acrolein or acrolein and acrylic acid in a heated, moving aqueous H2O2 solution and in the presence of about 0.1 to about 10.0 % by weight thioethylene glycol. The polycarboxylates are readily biodegradable rendering them especially suitable for use as phosphate substitutes in detergents and cleaning agents.
Inventors
- 👤 Heinz Haschke
- 👤 Gerhard Morlock
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 19:23
CPC Classifications
C; C08; C08F; C08F246/00; Y; Y10; Y10S; Y10S260/00; Y10S260/43
Claims Analysis
Total Claims: 26
Claim 1
Independent Claim
77 words
AN IMPROVED PROCESS FOR THE PREPARATION OF A POLYCARBOXYLATE BY THE OXIDATIVE POLYMERIZATION OF ACROLEIN OR ACROLEIN AND ACRYLIC ACID, SAID POLYCARBOXYLATE HAVING IMPROVED BIOLOGICAL DEGRADABILITY, SAID PROCESS COMPRISING SLOWLY ADDING ACROLEIN MONOMER OR AN ACROLEIN-ACRYLIC ACID MONOMER MIXTURE TO A HEATED, MOVING AQUEOUS HYDROGEN PEROXIDE SOLUTION, WHEREIN THE IMPROVEMENT COMPRISES CONDUCTING SAID POLYMERIZATION IN THE PRESENCE OF ABOUT 0.1 TO ABOUT 10% BY WEIGHT OF THIOETHYLENE GLYCOL, RELATED TO THE WEIGHT OF MONOMER OR MONOMER MIXTURE.
Claim 2
Dependent Claim
77 words
AN IMPROVED PROCESS FOR THE PREPARATION OF A POLYCARBOXYLATE BY THE OXIDATIVE POLYMERIZATION OF ACROLEIN OR ACROLEIN AND ACRYLIC ACID, SAID POLYCARBOXYLATE HAVING IMPROVED BIOLOGICAL DEGRADABILITY, SAID PROCESS COMPRISING SLOWLY ADDING ACROLEIN MONOMER OR AN ACROLEIN-ACRYLIC ACID MONOMER MIXTURE TO A HEATED, MOVING AQUEOUS HYDROGEN PEROXIDE SOLUTION, WHEREIN THE IMPROVEMENT COMPRISES CONDUCTING SAID POLYMERIZATION IN THE PRESENCE OF ABOUT 0.1 TO ABOUT 10% BY WEIGHT OF THIOETHYLENE GLYCOL, RELATED TO THE WEIGHT OF MONOMER OR MONOMER MIXTURE.
Claim 3
Dependent Claim
31 words
Process according to claim 1 in which at least part of the thioethylene glycol is added to the hydrogen peroxide solution simultaneously with the addition of the monomer or monomer mixture.
Claim 4
Dependent Claim
19 words
Process according to claim 1 in which the monomer mixture comprises up to about 50 mole % acrylic acid.
Claim 5
Dependent Claim
20 words
Process according to claim 3 in which the monomer mixture comprises about 10 to about 30 mole % acrylic acid.
Claim 6
Dependent Claim
19 words
Process according to claim 1 in which the solution comprises about 10 to about 35% by weight hydrogen peroxide.
Claim 7
Dependent Claim
17 words
Process according to claim 1 in which the solution is heated at about 55* to about 95*C.
Claim 8
Dependent Claim
51 words
Process according to claim 1 in which the solution is heated at about 65* to about 85*C. 8. Process according to claim 1 in which the acrolein and hydrogen peroxide are present in an amount such that there are about 1.0 to 1.2 moles of acrolein per mole of hydrogen peroxide.
Claim 9
Dependent Claim
23 words
Process according to claim 1 in which the monomer or monomer mixture is added within a time of up to about 7 hours.
Claim 10
Dependent Claim
24 words
Process according to claim 1 in which the monomer or monomer mixture is added over a period of about 3 to about 5 hours.
Claim 11
Dependent Claim
22 words
Process according to claim 1 in which the thioethylene glycol is in an amount of about 0.5 to about 5% by weight.
Claim 12
Dependent Claim
23 words
Process according to claim 1 in which the thioethylene glycol is employed in an amount of about 1 to about 2% by weight.
Claim 13
Dependent Claim
16 words
Process according to claim 1 in which the resulting polymerizate is subsequently subjected to Cannizzaro reaction.
Claim 14
Dependent Claim
16 words
Process according to claim 13 in which the polymerizate is reacted with an alkali metal hydroxide.
Claim 15
Dependent Claim
27 words
Process according to claim 1 in which the monomer or monomer mixture contains up to about 500 ppm of a stabilizer which will retard spontaneous radical polymerization.
Claim 16
Dependent Claim
14 words
Process according to claim 15 in which the stabilizer is a hydroquinone monomethyl ether.
Claim 17
Dependent Claim
23 words
Process according to claim 1 in which a lower alcohol or silicone-based defoaming agent is employed during polymerization in order to decrease foaming.
Claim 18
Dependent Claim
14 words
Process according to claim 14 in which the alkali metal is sodium or potassium.
Claim 19
Dependent Claim
56 words
Process according to claim 1 in which the resulting polymerizate is subsequently subjected to Cannizzaro reaction in a dilute solution of the resulting polymerizate or a dilute alkali metal hydroxide solution or by a slow addition of alkali metal hydroxide to an agitated solution of the resulting polymerizate in order to avoid localized condensation to aldols.
Claim 20
Dependent Claim
17 words
Process according to claim 19 in which Cannizzaro reaction is carried out in the presence of formaldehyde.
Claim 21
Dependent Claim
32 words
Process according to claim 1 in which, after completion of the addition of the monomers, the aqueous solution is stirred for up to about 12 hours at about 40* to about 90*C.
Claim 22
Dependent Claim
25 words
Process according to claim 21 in which said stirring is conducted at about 50* to about 75*C after completion of the addition of the monomers.
Claim 23
Dependent Claim
19 words
Process according to claim 1 in which unreacted monomers are removed from the solution by distillation or film evaporation.
Claim 24
Dependent Claim
26 words
Process according to claim 23 in which distillation is conducted at reduced pressure and about 10 to about 40% by volume of the solution is removed.
Claim 25
Dependent Claim
21 words
Process according to claim 5 in which the hydrogen peroxide solution comprises about 15 to about 25% by weight hydrogen peroxide.
Claim 26
Dependent Claim
24 words
Process according to claim 10 in which the monomer or monomer mixture is added over a period of about 2 to about 7 hours.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-12-01 | 1979-06-02 | 1979-12-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-12-01 | 1983-06-02 | 1983-12-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-12-01 | 1987-06-02 | 1987-12-02 | $7700.00 | Window Closed / Lapsed |