Process for making acrylamide

Claim 2

A PROCESS FOR CATALYTICALLY HYDROOLYZING ACRYLONITRILE TO ACRYLAMIDE COMPRISING THE STEPS OF SEQUENTIALLY A. SUSPENDING IN WATER CONTAINED IN A REACTION ZONE WITH AGITATION COPPER CATALYST PARTICLES HAVING A STANDARDIZED NITRILE HYDROLYSIS ACTIVITY OF AT LEAST ABOUT 50 WEIGHT PERCENT AND FURTHER HAVING A PARTICLE SIZE RANGING FROM ABOUT 0.002 TO 0.1 INCHES IN AVERAGE DIAMEERS, THE WEIGHT RATIO OF SAID WATER TO SAID CATALYT RANGING FRO ABOUT 0.02 TO 0.20, B. ADDING TO SAID WATER WHILE SAID CATALYST PARTICLES ARE SUSPENDED THEREIN AT AN INTIAL WATER TEMPERATURE RANGING FROM ABOUT 180* TO 30*F INCREMENTALLY ACRYLONITRILE WITH AGITATION, THE RATE OF SAID INCREMENTALLY ACRYLONITRILE WITH TEMPERATURE OF SAID WATER IS MAINTAINED IN THE RANGE OF FROM ABOUT 180* TO 300*F., THE TOTAL AMOUNT OF ACRYLONITRILE SO ADDED BEING SUCH THAT THE WEIGHT RATIO OF SAID WATER TO SAID TOTAL ACRYLONITRILE RANGES FROM ABOUT 50:50 TO 75.25, SAID RATE OF ADDITION BEING SUCH AS TO PRODUCE A TOTAL CONVERSION OF ACRYLONITIRILE TO ACRYLAMIDE IN SAID REACTION ZONE OF AT LEAST ABOUT 45% AT THE TIME WHEN SAID ADDING IS COMPLETED, C. MAINTAINING THE RESULTING MIXTURE IN SAID REACTION ZONE WITH AGITATION AT A WATER TEMPERATURE RANGING FROM ABOUT 180* TO 3300*F UNTIL THE TOTAL CONVERSATION OF SAID ACRYLONITRILE TO PRODUCED ACRYLAMIDE IS AT LEAST ABOUT 65%, D. TERMINATING SAID AGITATION IN SAID REACTION ZONE, THEREBY CAUSING SAID CATALYST PARTICLES TO ALL TO THE BOTTOM OF SAID REACTION ZONE, E. REMOVING AT LEAST A MAJOR PORTION OF SAID ACRYLAMIDE PRODUCT SOLUTION FROM SAID REACTION ZONE WHILE RETAINING SUBSTANTIALLY ALL OF SAID CATALYST PARTICLES IN SAID REACTION ZONE,

Claim 3

The process of claim 1 wherein said steps (A) through (F) are so sequentially repeated at least 5 times.

Claim 4

The process of claim 1 wherein said steps (A) through (F) are so sequentially repeated at least 10 times.

Claim 5

The process of claim 1 wherein said steps (A) through (F) are so sequentially repeated at least 15 times.

Claim 6

The process of claim 1 wherein the cycle time for steps (A) through (F) ranges from about 4 through 40 hours.

Claim 7

The process of claim 1 wherein the rate of addition of said acrylonitrile is such that steps (B) and (C) are practiced simultaneously and the total conversion of acrylonitrile to acrylamide in said raction zone is at least about 65%.

Claim 8

THE PROCESS OF CLAIM 1 WHEREIN INTIALLY PRIOR TO STEP (A) SAID PROCESS COMPRISES THE STEP OF A. CHARGING WATER TO SAID REACTION ZONE, B. CHARGING AN ALLOY COMPRISING COPPER AND ALUMINIM IN A WEIGHT RATIO OF FROM ABOUT 30.70 TO 70.30 COPPER TO ALUMINUM IN THE FORM OF PARTICLES HAVING A SIZE RANGING FROM ABOUT 0.002 TO 0.1 INCHES IN AVERAGE MAXIMUM DIAMETER TO SAID REACTION ZONE TO PRODUCE AN INITIAL WEIGHT RATIO OF SAID ALLOY PARTICCLES TO SAID WATER IN THE RANGE FROM ABOUT 0.01 TO 0.35, C. SUSPENDING SAID ALLOY PARTICLES IN SAID WATER WITH AFITATION, D. ADDING ALKALI METAL HYDROXIDE TO SUCH SUSPENSION WHILE MAINTAINING THE BULK TEMPERATURE OF SAID WATER IN THE RANGE FROM ABOUT 32O TO 180*F., THE TOTAL QUANTITY OF ALKALI METAL HYROOXIDE CHARGED TO SUCH SUSPENSION RANGING FROM ABOUT 0.5 TO 20 TIMES THE NUMBER OF MOLES OF ALUMINUM, INTIALLY PRESENT IN SAID ALLOY, THE TOTAL TIME OF SUCH ADDING RANGING FROM ABOUT 2 TO 50 HOURS, E. TERMINATIN SAID AGITATION IN SAID REACTION ZONE, THEREBY CAUSING SAID CATALYST PARTICLES TO FALL TO THE BOTTOM OF SAID REACTION ZONE, F. REMOVING SAID WATER WITH SAID ALKALI METAL HYDROXIDE CONTAINED THEREIN, AND G. WASHING WITH WATER SAID CATALYST PARTICLS UNTIL A WASH WATER PH NOT ABOVE 8.0 IS ACHIVED.

Claim 9

The process of claim 7 wherein after said adding is completed, the resulting solution of alkali metal hydroxide is maintained in contact with said particles while so suspended until at least about 35 weight percent of said aluminum initially present in said alloy on a 100 weight percent total initial alloy basis is removed thereby to produce catalyst particles from said alloy particles.

Claim 10

A process for catalytically hydrolyzing acrylonitrile to acrylamide comprising the steps of sequentially A. suspending in water contained in a reaction zone with agitation Raney copper catalyst particles having a standardized nitrile hydrolysis activity of from about 70 to 95 weight percent and further having a particle size ranging from about 0.005 to 0.02 inches in average diameters, the weight ratio of said catalyst to said water ranging From about 0.05 to 0.1, B. adding incrementally to said water acrylonitrile, while said catalyst particles are suspended therein at an initial water temperature ranging from about 200* to 250* F, the rate of said addition being such that the temperature of said water is maintained in the range of from about 200* to 250* F., the total amount of acrylonitrile so added being such that the weight ratio of said water to said total acrylonitrile ranges from about 60:40 to 70:30, said rate of addition being such as to produce a total conversion of acrylonitrile to acrylamide in said reaction zone of at least about 60% at the time when said adding is completed, C. maintaining the resulting mixture in said reaction zone with agitation at a water temperature ranging from about 180* to 300* F. until the total conversion of said acrylonitrile to produced acrylamide is at least about 80%, D. terminating said agitation in said reaction zone, thereby causing said catalyst particles to fall to the bottom of said reaction zone, E. removing at least a major portion of said acrylamide product solution from said reaction zone while retaining substantially all of said catalyst particles in said reaction zone, F. charging water to said reaction zone in an amount sufficient to bring the weight ratio of said catalyst to said water into said range of from about 0.05 to 0.1, G. repeating sequentially steps (A) through (F).

Claim 11

A process for catalytically hydrolyzing acrylonitrile to acrylamide comprising the steps of sequentially A. suspending in water contained in a reaction zone with agitation Raney copper catalyst particles having a standardized nitrile hydrolysis activity of from about 70 to 95 weight percent and further having a particle size ranging from about 0.005 to 0.02 inches in average diameters, the weight ratio of said catalyst to said water ranging From about 0.05 to 0.1, B. adding incrementally to said water acrylonitrile, while said catalyst particles are suspended therein at an initial water temperature ranging from about 200* to 250* F, the rate of said addition being such that the temperature of said water is maintained in the range of from about 200* to 250* F., the total amount of acrylonitrile so added being such that the weight ratio of said water to said total acrylonitrile ranges from about 60:40 to 70:30, said rate of addition being such as to produce a total conversion of acrylonitrile to acrylamide in said reaction zone of at least about 60% at the time when said adding is completed, C. maintaining the resulting mixture in said reaction zone with agitation at a water temperature ranging from about 180* to 300* F. until the total conversion of said acrylonitrile to produced acrylamide is at least about 80%, D. terminating said agitation in said reaction zone, thereby causing said catalyst particles to fall to the bottom of said reaction zone, E. removing at least a major portion of said acrylamide product solution from said reaction zone while retaining substantially all of said catalyst particles in said reaction zone, F. charging water to said reaction zone in an amount sufficient to bring the weight ratio of said catalyst to said water into said range of from about 0.05 to 0.1, G. repeating sequentially steps (A) through (F).

Claim 12

The process of claim 9 wherein said steps (A) through (F) are so sequentially repeated at least 5 times.

Claim 13

The process of claim 9 wherein said steps (A) through (F) are so sequentially repeated at least 10 times.

Claim 14

The process of claim 9 wherein said steps (A) through (F) are so sequentially repeated at least 15 times.

Claim 15

The process of claim 9 wherein the cycle time for steps (A) through (F) ranges from about 8 through 20 hours.

Claim 16

The process of claim 9 wherein the rate of addition of said acrylonitrile is such that steps (B) and (C) are practiced simultaneously and the total conversion of acrylonitrile to acrylamide in said reaction zone is at least about 80%.

Claim 17

The process of claim 9 wherein initially prior to step (A) said process comprises the steps of A. charging water to said reaction zone, B. charging an alloy comprising copper and aluminum in a weight ratio of from about 40:60 to 60:40 copper to aluminum in the form of particles having a size ranging from about 0.005 to 0.02 inches in average maximum diameter to said reaction zone to produce an initial weight ratio of said alloy particles to said water in the range from about 0.01 to 0.35, C. suspending said alloy particles in said water with agitation, D. adding alkali metal hydroxide to such suspension while maintaining the bulk temperature of said water in the range from about 60* to 120* F., the total quantity of alkali metal hydroxide charged to such suspension ranging from about 1.0 to 3.0 times the number of moles of aluminum initially present in said alloy, the total time of such adding ranging from about 4 to 40 hours, E. terminating said agitation in said reaction zone, thereby causing said catalyst particles to fall to the bottom of said reaction zone, F. removing said water with said alkali metal hydroxide contained therein, and G. washing with water said catalyst particles until a wash water pH not above about 8.0 is achieved.

Claim 18

The process of claim 15 wherein after said adding is completed, the resulting solution of alkali metal hydroxide is maintained in contact with said particles while so suspended until at least about 80 weight percent of said aluminum initially present in said alloy on a 100 weight percent totAl initial alloy basis is removed thereby to produce catalyst particles from said alloy particles.