calcium;propanoate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This invention relates to a process for recovering calcium formate, propionate or acetate from biomass. According to the invention, a cellulose-, hemicellulose- or starch-containing biomass is subjected to rapid pyrolysis to obtain a crude product containing an aqueous phase and an organic phase. The product obtained, preferably as the aqueous phase, is then distilled to produce a distillate containing at least one acid selected from acetic acid, formic acid and propionic acid as well as their esters and formaldehyde. An alkaline source of calcium is added to this distillate to adjust the pH to an alkaline level sufficient to hydrolyze the esters, cause at least partial oxidation of the formaldehyde and prevent volatilization of acetate, formate or propionate ions as acetic acid, formic acid or propionic acid respectively. For this purpose, the pH is adjusted to a level sufficient to prevent volatilization of acetate, formate or propionate as acetic acid, formic acid or propionic acid respectively. The pH is preferably above 7, but preferably sufficiently low as to avoid residual unreacted alkaline calcium in the calcium salt. A pH range of 7.8 to 8.0 is particularly preferred. This pH adjusted alkaline liquid is then subjected to a further distillation to remove water and volatile organic components and produce at least one of calcium acetate, calcium formate and calcium propionate as solid residue. containing an aqueous phase The product obtained, preferably as the aqueous phase is then distilled to produce a distillate containing at least one acid is then subjected to a further distillation to remove water and volatile organic components

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This invention relates to a process for recovering calcium formate, propionate or acetate from biomass. According to the invention, a cellulose-, hemicellulose- or starch-containing biomass is subjected to rapid pyrolysis to obtain a crude product containing an aqueous phase and an organic phase. The product obtained, preferably as the aqueous phase, is then distilled to produce a distillate containing at least one acid selected from acetic acid, formic acid and propionic acid as well as their esters and formaldehyde. An alkaline source of calcium is added to this distillate to adjust the pH to an alkaline level sufficient to hydrolyze the esters, cause at least partial oxidation of the formaldehyde and prevent volatilization of acetate, formate or propionate ions as acetic acid, formic acid or propionic acid respectively. For this purpose, the pH is adjusted to a level sufficient to prevent volatilization of acetate, formate or propionate as acetic acid, formic acid or propionic acid respectively. The pH is preferably above 7, but preferably sufficiently low as to avoid residual unreacted alkaline calcium in the calcium salt. A pH range of 7.8 to 8.0 is particularly preferred. This pH adjusted alkaline liquid is then subjected to a further distillation to remove water and volatile organic components and produce at least one of calcium acetate, calcium formate and calcium propionate as solid residue. containing an aqueous phase The product obtained, preferably as the aqueous phase is then distilled to produce a distillate containing at least one acid is then subjected to a further distillation to remove water and volatile organic components

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Calcium salts, such as calcium acetate, calcium formate or calcium proprionate, are obtained from aqueous liquors derived from the pyrolysis of lignocellulosic biomass containing cellulose, hemicelluloses or starch. The above biomass is subjected to rapid pyrolysis to obtain a crude product containing an aqueous phase and an organic phase. The product obtained, preferably as the aqueous phase, is then distilled to produce a distillate containing at least one acid selected from acetic acid, formic acid and propionic acid as well as their esters and formaldehyde. An alkaline source of calcium is added to this distillate to adjust the pH to an alkaline level sufficient to hydrolyze the esters, cause at least partial oxidation of the formaldehyde and prevent volatilization of acetate, formate or propionate ions as acetic acid, formic acid or propionic acid respectively. This pH adjusted alkaline liquid is then subjected to a further distillation to remove water and volatile organic components and produce at least one of calcium acetate, calcium formate and calcium propionate as solid residue. to obtain a crude product containing an aqueous phase The product obtained, preferably as the aqueous phase is then distilled to produce a distillate containing at least one acid is then subjected to a further distillation to remove water and volatile organic components

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Calcium salts, such as calcium acetate, calcium formate or calcium proprionate, are obtained from aqueous liquors derived from the pyrolysis of lignocellulosic biomass containing cellulose, hemicelluloses or starch. The above biomass is subjected to rapid pyrolysis to obtain a crude product containing an aqueous phase and an organic phase. The product obtained, preferably as the aqueous phase, is then distilled to produce a distillate containing at least one acid selected from acetic acid, formic acid and propionic acid as well as their esters and formaldehyde. An alkaline source of calcium is added to this distillate to adjust the pH to an alkaline level sufficient to hydrolyze the esters, cause at least partial oxidation of the formaldehyde and prevent volatilization of acetate, formate or propionate ions as acetic acid, formic acid or propionic acid respectively. This pH adjusted alkaline liquid is then subjected to a further distillation to remove water and volatile organic components and produce at least one of calcium acetate, calcium formate and calcium propionate as solid residue. to obtain a crude product containing an aqueous phase The product obtained, preferably as the aqueous phase is then distilled to produce a distillate containing at least one acid is then subjected to a further distillation to remove water and volatile organic components

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: About 70 g of calcium propionate-propionic acid is dissolved in 30 g of water to yield a 70 percent solution by weight of dissociated calcium propionate and propionic acid.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This invention relates to a process for recovering calcium formate, propionate or acetate from biomass. According to the invention, a cellulose-, hemicellulose- or starch-containing biomass is subjected to rapid pyrolysis to obtain a crude product containing an aqueous phase and an organic phase. The product obtained, preferably as the aqueous phase, is then distilled to produce a distillate containing at least one acid selected from acetic acid, formic acid and propionic acid as well as their esters and formaldehyde. An alkaline source of calcium is added to this distillate to adjust the pH to an alkaline level sufficient to hydrolyze the esters, cause at least partial oxidation of the formaldehyde and prevent volatilization of acetate, formate or propionate ions as acetic acid, formic acid or propionic acid respectively. For this purpose, the pH is adjusted to a level sufficient to prevent volatilization of acetate, formate or propionate as acetic acid, formic acid or propionic acid respectively. The pH is preferably above 7, but preferably sufficiently low as to avoid residual unreacted alkaline calcium in the calcium salt. A pH range of 7.8 to 8.0 is particularly preferred. This pH adjusted alkaline liquid is then subjected to a further distillation to remove water and volatile organic components and produce at least one of calcium acetate, calcium formate and calcium propionate as solid residue. containing an aqueous phase The product obtained, preferably as the aqueous phase is then distilled to produce a distillate containing at least one acid is then subjected to a further distillation to remove water and volatile organic components

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Calcium salts, such as calcium acetate, calcium formate or calcium proprionate, are obtained from aqueous liquors derived from the pyrolysis of lignocellulosic biomass containing cellulose, hemicelluloses or starch. The above biomass is subjected to rapid pyrolysis to obtain a crude product containing an aqueous phase and an organic phase. The product obtained, preferably as the aqueous phase, is then distilled to produce a distillate containing at least one acid selected from acetic acid, formic acid and propionic acid as well as their esters and formaldehyde. An alkaline source of calcium is added to this distillate to adjust the pH to an alkaline level sufficient to hydrolyze the esters, cause at least partial oxidation of the formaldehyde and prevent volatilization of acetate, formate or propionate ions as acetic acid, formic acid or propionic acid respectively. This pH adjusted alkaline liquid is then subjected to a further distillation to remove water and volatile organic components and produce at least one of calcium acetate, calcium formate and calcium propionate as solid residue. to obtain a crude product containing an aqueous phase The product obtained, preferably as the aqueous phase is then distilled to produce a distillate containing at least one acid is then subjected to a further distillation to remove water and volatile organic components

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 186 g (1 mol) of calcium propionate are dissolved in 500 ml of water. To this solution are added, at 25° C., a solution of 56 g (0.37 mol) of potassium sorbate in 60 ml of water. During addition a precipitate forms which is filtered off after 2 min. The precipitate is dried to constant weight at 150 mbar and 50° C. 90% pure calcium propionate sorbate is obtained as a white powder in 75% yield. To this solution are added, at 25° C. During addition a precipitate forms which is filtered off after 2 min The precipitate is dried to constant weight at 150 mbar and 50° C

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A process for producing a calcium propionate comprising contacting propionitrile, a calcium compound selected from calcium hydroxide, calcium oxide or mixtures thereof, and water at a temperature of about 90° C. to about 250° C. at a sufficient pressure to achieve the desired temperature and for a sufficient time to produce a reaction mixture comprising calcium propionate; at a temperature of about 90° C. to about 250° C.

反応条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Propionitrile (311.5 g, 5.66 mol, supplied by Solutia Inc., refined: 99.6% min) was charged into a one gallon 316 stainless steel autoclave through a funnel. Calcium hydroxide (229.3 g, 3.09 mol, supplied by Mississippi Lime, CODEX Hydrated Lime), and deionized water (1007.2 g, 55.9 mol) were mixed to produce a slurry and charged to the autoclave through the same funnel. A second portion of deionized water (345.1 g, 19.2 mol) was used to rinse the calcium hydroxide slurry container and was charged to the autoclave through the funnel. The autoclave was pressurized with nitrogen to 45-55 psig (310.3-379.2 KPa), and the pressure relieved to under 25 psig (172.4 KPa). This cycle was repeated two additional times to purge most of the air from the system. The pressure control valve was set to 260 psig (1792.6 KPa), and a nitrogen flow (100 std cm3/min) through the reactor vapor space was started. The autoclave agitator was started and the contents were heated to 200° C. with a mixture of steam and water under pressure in an internal coil. After the autoclave contents had been at 200° C. for one hour, the nitrogen flow was increased to 200 cm3/min to improve the control of the autoclave pressure. After the autoclave contents had been at 200° C. for a total of two hours, the steam was turned off and the reactor pressure was released through a vapor line heated to over 200° C. over a period of 40 minutes. The water and ammonia that flashed from the autoclave was trapped by passing it into a scrubber containing 4862.6 grams of ice water. This scrubber solution weighed 5414.9 grams after all of the autoclave pressure had been released. After the autoclave contents had cooled to less than 60° C. they were drained and weighed (925.1 g). Deionized water (237.2 g) was added to dissolve all of the calcium propionate. This diluted product was analyzed by the HPLC method described in Example 1 and found to contain 28.0% calcium propionate (326 g, 1.75 mol, 62% yield), 119 ppm of propionamide, and no detectable propionitrile. The scrubber solution was found to contain 0.34% calcium propionate and 1.58% ammonia. From the amount of calcium propionate in the scrubber, it was concluded that approximately 66.4 grams of the product was carried into the scrubber by entrainment and that 400 grams of water and 85.5 grams of ammonia were flashed from the autoclave. This represents 90% of the ammonia that would be expected from complete hydrolysis of the propionitrile charged to the autoclave. No attempt was made to quantify the amount of calcium propionate remaining in the reactor after the product was drained. to produce a slurry charged to the autoclave through the same funnel to rinse the calcium hydroxide slurry container was charged to the autoclave through the funnel to purge most of the air from the system the nitrogen flow was increased to 200 cm3/min had been at 200° C. for a total of two hours heated to over 200° C. over a period of 40 minutes containing 4862.6 grams of ice water After the autoclave contents had cooled to less than 60° C. they Deionized water (237.2 g) was added to dissolve all of the calcium propionate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The experiment was repeated using 30 g of 80% propionic acid, 10.81 g of calcium hydroxide and 0.91 g or calcium oxide. A non-dusty product without lumps was formed. A non-dusty product without lumps was formed

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: About 70 g of calcium propionate-propionic acid is dissolved in 30 g of water to yield a 70 percent solution by weight of dissociated calcium propionate and propionic acid.