US3911048A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for the continuous preparation of unsaturated polyesters
Assignee: Societa Italiana Resine SpA SIR
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Filing: 1973-11-29
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Granted: 1975-10-07
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Expires: 1993-11-29
Abstract
Abstract Process for the continuous preparation of unsaturated polyesters, comprising bringing olefinically unsaturated dicarboxylic acids or their anhydrides, if desired, together with saturated dicarboxylic acids of their anhydrides (dicarboxylic acid component) and dihydric alcohols, if desired, together with higher polyhydric alcohols (alcohol component) into contact in molar ratios of from about 1.5:1 to 1.95:1 in a first reaction phase, operating at a temperature of from about 100* to 160*C and with residence times of from about 5 to 40 minutes to cause the formation of a corresponding half-ester; adding to the half-ester formed a further quantity of the alcohol component in such a way as to give a molar ratio of the dicarboxylic acid component to the total amount of the alcohol component in the range of from about 0.87:1 to 0.97:1; bringing about the polyesterification in a second reaction phase by treating the product obtained in at least two separate and successive stages, which are operated at decreasing pressure values in the range of from about 5 atmospheres to atmospheric pressure, for times of about 2 to 8 hours, and at temperatures of from about 100* to 220*C, the temperature in said stages not differing by more than about 10*C, and the water formed during the polyesterification being eliminated from each of the said stages; evaporating the residual water and the excess of the alcohol component from the polyesterification product obtained with operation at pressures below atmospheric pressure.
Inventors
- 👤 Silvio Vargiu
- 👤 Beppino Passalenti
- 👤 Ugo Nistri
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 08:54
CPC Classifications
C; C08; C08G; C08G63/00; C08G63/02; C08G63/12; C08G63/52; C08G63/78; C08G63/785
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
253 words
A process for the continuous production of unsaturated polyesters, which comprises the steps of a. bringing olefinically unsaturated dicarboxylic acids or their anhydrides, if desired together with saturated dicarboxylic acids or their anhydrides (dicarboxylic acid component) and dihydric alcohols, if desired together with higher polyhydric alcohols (alcohol component) into contact in molar ratios of from about 1.5:1 to 1.95:1 in a first reaction phase, operating at a temperature of from about 100* to 160*C and with residence times of from about 5 to 40 minutes to cause the formation of a corresponding half-ester; b. adding to the half-ester formed a further quantity of the alcohol component in such a way as to give a molar ratio of the dicarboxylic acid component to the total amount of the alcohol component in the range of from about 0.87:1 to 0.97:1; c. bringing about the polyesterification in a second reaction phase by treating the product obtained in b) in at least two separate and successive stages, which are operated at decreasing pressure values in the range of from about 5 atmospheres to atmospheric pressure, for a total time of from about 2 to 8 hours, and at temperatures of from about 100* to 220*C, the temperature between said stages not differing by more than about 10*C, the water formed during the polyesterification being eliminated from each of the said stages; d. evaporating the residual water and the excess of the alcohol component from the polyesterification product obtained in c) with operation at pressures below atmospheric pressure.
Claim 2
Dependent Claim
253 words
A process for the continuous production of unsaturated polyesters, which comprises the steps of a. bringing olefinically unsaturated dicarboxylic acids or their anhydrides, if desired together with saturated dicarboxylic acids or their anhydrides (dicarboxylic acid component) and dihydric alcohols, if desired together with higher polyhydric alcohols (alcohol component) into contact in molar ratios of from about 1.5:1 to 1.95:1 in a first reaction phase, operating at a temperature of from about 100* to 160*C and with residence times of from about 5 to 40 minutes to cause the formation of a corresponding half-ester; b. adding to the half-ester formed a further quantity of the alcohol component in such a way as to give a molar ratio of the dicarboxylic acid component to the total amount of the alcohol component in the range of from about 0.87:1 to 0.97:1; c. bringing about the polyesterification in a second reaction phase by treating the product obtained in b) in at least two separate and successive stages, which are operated at decreasing pressure values in the range of from about 5 atmospheres to atmospheric pressure, for a total time of from about 2 to 8 hours, and at temperatures of from about 100* to 220*C, the temperature between said stages not differing by more than about 10*C, the water formed during the polyesterification being eliminated from each of the said stages; d. evaporating the residual water and the excess of the alcohol component from the polyesterification product obtained in c) with operation at pressures below atmospheric pressure.
Claim 3
Dependent Claim
35 words
The process of claim 1, wherein the polyesterification is carried out in 3 to 4 reaction stages, with a pressure that decreases in the various stages from about 3 to 4 atmospheres to atmospheric pressure.
Claim 4
Dependent Claim
35 words
The process of claim 1, wherein the evaporation in step d) is carried out by a thin-film technique at pressures of from about 2 to 50 mmHg and at temperatures not exceeding the polyesterification temperatures.
Claim 5
Dependent Claim
23 words
The process of claim 1, wherein as olefinically unsaturated dicarboxylic acid components maleic acid and its anhydride, itaconic or fumaric acid are used.
Claim 6
Dependent Claim
31 words
The process of claim 1, wherein as saturated dicarboxylic acid components succinic acid and its anhydride, sebacic acid, phthalic acid and its anhydride, and isophthalic, terephthalic or adipic acid are used.
Claim 7
Dependent Claim
28 words
The pRocess of claim 1, wherein as dihydric alcohol components 1,2-propylene glycol, ethylene glycol, diethylene glycol, triethylene glycol, butylene glycol, dipropylene glycol, 1,6-hexanediol or neopentyl glycol are used.
Claim 8
Dependent Claim
17 words
The process of claim 1, wherein maleic acid anhydride, phthalic acid anhydride and 1,2-propylene glycol are used.
Claim 9
Dependent Claim
275 words
IN A PROCESS FOR PRODUCING UNSATURATED POLYESTER MIXTURES CONSISTING OF MIXING UNSATURATED POLYESTERS WITH AT LEAST ON POLYMERIZABLE MONOMERIC ACRYLIC OR VINYL COMPOUND THE IMPROVEMENT WHICH COMPRISES CONTINUOUSLY PRODUCING SAID UNSATURATED POLYESTERS BY THE STEPS OF: A. BRINGING OLEFINICALLY UNSATURATED DICARBOXYLIC ACIDS OR THEIR ANHYDRIDES, IF DESIRED TOGETHER WITH SATURATED DICARBOXYLIC ACIDS OR THEIR ANHYDRIDES (DICARBOXYLIC ACID COMPONENT) AND DIHYDRIC ALCOHOLS, IF DESIRED TOGETHER WITH HIGHER POLYHYDRIC ALCOHOLS (ALCOHOL COMPONENT) INTO CONTACT IN MOLAR RATIOS OF FROM ABOUT 1.5:1 TO 1.95:1 IN A FIRST PHASE, OPERATING AT A TEMPERATURE OF FROM ABOUT 100* TO 160*C AND WITH RESIDENCE TIMES OF FROM ABOUT 5 TO 40 MINUTES TO CAUSE THE FROMATION OF A CORESPONDING HALF-ESTER, B. ADDING TO THE HALF-ESTER FORMED A FURTHER QUANTITY OF THE ALCOHOL COMPONENT IN SUCH A WAY AS TO GIVE A MOLAR RATIO OF THE DICARBOXYLIC ACID COMPONENT TO A TOTAL AMOUNT OF THE ALCOHOL COMPONENT IS THE RANGE OF FROM ABOUT 0.87:1 TO 0.97:1, C. BRINGING ABOUT THE POLYESTERIFICATION IN A SECOND REACTION PHASE BY THE TREATING PRODUCT OBTAIN IN B) IN AT LEAST TWO SEPARATE AND SUCCESSIVE STAGES, WHICH ARE OPERATED AT DECREASING PRESSURE VALUES IN THE RANGE OF FROM ABOUT 5 ATMOSPHERES TO ATMOSPHERIC PRESSURE, FOR A TOTAL TIME OF FROM ABOUT 2 TO 8 HOURS, AND AT A TEMPERATURES OF FROM ABOUT 100* TO 220*C, THE TEMPERATURE BETWEEN SAID STAGES NOT DIFFERING BY MORE THAN ABOUT 10*C, THE WATER FORMED DURING THE POLYESTERIFICATION BEING ELIMINATED FROM EACH OF THE SAID STAGES, D. EVAPORATING THE RESIDUAL WATER AND THE EXCESS OF THE ALCOHOL COMPONENT FROM THE POLYESTERIFICATION PRODUCT OBTAINED IN C) WITH OPERATION AT PRESSURES BELOW ATMOSPHERIC PRESSURE.
Claim 10
Dependent Claim
275 words
IN A PROCESS FOR PRODUCING UNSATURATED POLYESTER MIXTURES CONSISTING OF MIXING UNSATURATED POLYESTERS WITH AT LEAST ON POLYMERIZABLE MONOMERIC ACRYLIC OR VINYL COMPOUND THE IMPROVEMENT WHICH COMPRISES CONTINUOUSLY PRODUCING SAID UNSATURATED POLYESTERS BY THE STEPS OF: A. BRINGING OLEFINICALLY UNSATURATED DICARBOXYLIC ACIDS OR THEIR ANHYDRIDES, IF DESIRED TOGETHER WITH SATURATED DICARBOXYLIC ACIDS OR THEIR ANHYDRIDES (DICARBOXYLIC ACID COMPONENT) AND DIHYDRIC ALCOHOLS, IF DESIRED TOGETHER WITH HIGHER POLYHYDRIC ALCOHOLS (ALCOHOL COMPONENT) INTO CONTACT IN MOLAR RATIOS OF FROM ABOUT 1.5:1 TO 1.95:1 IN A FIRST PHASE, OPERATING AT A TEMPERATURE OF FROM ABOUT 100* TO 160*C AND WITH RESIDENCE TIMES OF FROM ABOUT 5 TO 40 MINUTES TO CAUSE THE FROMATION OF A CORESPONDING HALF-ESTER, B. ADDING TO THE HALF-ESTER FORMED A FURTHER QUANTITY OF THE ALCOHOL COMPONENT IN SUCH A WAY AS TO GIVE A MOLAR RATIO OF THE DICARBOXYLIC ACID COMPONENT TO A TOTAL AMOUNT OF THE ALCOHOL COMPONENT IS THE RANGE OF FROM ABOUT 0.87:1 TO 0.97:1, C. BRINGING ABOUT THE POLYESTERIFICATION IN A SECOND REACTION PHASE BY THE TREATING PRODUCT OBTAIN IN B) IN AT LEAST TWO SEPARATE AND SUCCESSIVE STAGES, WHICH ARE OPERATED AT DECREASING PRESSURE VALUES IN THE RANGE OF FROM ABOUT 5 ATMOSPHERES TO ATMOSPHERIC PRESSURE, FOR A TOTAL TIME OF FROM ABOUT 2 TO 8 HOURS, AND AT A TEMPERATURES OF FROM ABOUT 100* TO 220*C, THE TEMPERATURE BETWEEN SAID STAGES NOT DIFFERING BY MORE THAN ABOUT 10*C, THE WATER FORMED DURING THE POLYESTERIFICATION BEING ELIMINATED FROM EACH OF THE SAID STAGES, D. EVAPORATING THE RESIDUAL WATER AND THE EXCESS OF THE ALCOHOL COMPONENT FROM THE POLYESTERIFICATION PRODUCT OBTAINED IN C) WITH OPERATION AT PRESSURES BELOW ATMOSPHERIC PRESSURE.
Claim 11
Dependent Claim
30 words
The process of claim 8, wherein the monomeric acrylic or vinyl compound is used in a quantity of from about 20 to 60 percent by weight on the unsaturated polyester.
Claim 12
Dependent Claim
12 words
The process of claim 9, wherein the monomeric vinyl compound is styrene.
References Cited (Backward Citations)
US3252941A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-10-06 | 1979-04-07 | 1979-10-07 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-10-06 | 1983-04-07 | 1983-10-07 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-10-06 | 1987-04-07 | 1987-10-07 | $7700.00 | Window Closed / Lapsed |