342 results about "Glufosinate" patented technology

The invention discloses a process for purifying glufosinate-ammonium, which comprises: (1) adding glufosinate-ammonium hydrochloride into an alcohol R1OH to perform an esterification reaction, and after the reaction is accomplished, cooling, filtering, removing solvent from filtrate and obtaining ester product of glufosinate-ammonium; (2) adding the ester product of glufosinate-ammonium, which isobtained by step (1), into water solution of hydrochloric acid to perform a hydrolysis reaction, and obtaining glufosinate-ammonium hydrochloride by post treatment; (3) adding the glufosinate-ammonium hydrochloride obtained by the step (2) into an alcohol R2OH, introducing epoxy ethane and obtaining glufosinate-ammonium acid; and (4) adding the glufosinate-ammonium acid obtained by the step (3) into an alcohol R3OH, introducing ammonia gas, and obtaining glufosinate-ammonium after the reaction is finished. In the invention, the process for purifying glufosinate-ammonium comprises simple steps, the inorganic salt content in the obtained glufosinate-ammonium is low, and the purity of the obtained glufosinate-ammonium is high; the process for separating glufosinate-ammonium hydrochloride from HCl by epoxy ethane is more economic than the conventional process which adopts epoxypropane and epoxy chloropropane; and the method is very safe and has a very bright industrialization prospect.

The invention discloses herbicide containing glufosinate. The herbicide containing glufosinate is characterized by comprising technical material composed of glufosinate and herbicide B according to a proportion of 1-80:1-80. The herbicide B is one of fenoxaprop-ethyl, fenoxaprop-P-ethyl, isoproturon, diclofop-methyl, chlortoluron, methabenzthiazuron, imazamethabenz, tralkoxydim, difenzoquat, flampro, flamprop-M, pendimethalin, nicosulfuron, primisulfuron and the like. The herbicide containing glufosinate is composed of herbicide A and the herbicide B and has the advantages that the herbicide is capable of killing ground weeds and grass seeds which are about to germinate and is long in effect duration; herbicide controlling spectrum is wide, and the herbicide is widely applicable to controlling weeds in dry lands; the herbicide is low in toxicity, weak in sensitization and low in poisoness to crops and human, can control weeds safely without harming the crops, and is evident in weed control synergy.

The invention discloses a production method of L-glufosinate. The method includes the steps that with 2-carbonyl-4-(hydroxyl methyl phosphoryl) butyric acid and salt thereof being a substrate, isolated transaminase or a cell catalysis substrate of in-vitro expression transaminase reacts with an amino donor under the condition that the amino donor exists, so that L-glufosinate is obtained, wherein the amino donor is alanine, and the amino acid sequence of transaminase is shown in SEQ ID NO.1-3. With 2-carbonyl-4-(hydroxyl methyl phosphoryl) butyric acid and salt thereof being the substrate and alanine being the amino donor, the transamination reaction occurs through the specific transaminase catalysis substrate, the substrate can be completely converted into L-glufosinate, and the conversion rate of raw materials is high and can reach 100%.

The invention discloses an enzyme-chemocatalysis racemization removing preparation method for L-glufosinate-ammonium. According to the method, a one-pot reaction manner is adopted, under the molecular oxygen, immobilization D-amino acid oxidase catalyzes D-enantiomer in an enantioselectivity mode into 2-imino-4-(hydroxy methyl phosphonyl) butyric acid in a dehydrogenation mode, and palladium-ammonium formate catalyzes 2-imino -4-(hydroxy methyl phosphonyl) butyric acid into DL-glufosinate-ammonium in an in-situ reduction mode. Hydrogen peroxide produced in the process is efficiently decomposed into water and oxygen through catalase. Complete reacemization removing of DL-glufosinate-ammonium and efficient preparing of L-glufosinate-ammonium are achieved through biological oxidation-chemical reduction circulation. The method has the advantages that the process is simple, cost is low, environmental friendliness is achieved, and energy is saved. High-concentration DL-glufosinate-ammonium can be converted into L-glufosinate-ammonium. The yield is 90%, the optical purity of the product is 99%, and the method is suitable for industrial production of L-glufosinate-ammonium.

The invention discloses a glufosinate-aryloxyphenoxypropionic acid herbicide weeding composition. The glufosinate-aryloxyphenoxypropionic acid herbicide weeding composition comprises glufosinate and an aryloxyphenoxypropionic acid herbicide as active ingredients, and the balance pesticide assistants. A weight ratio of glufosinate to the aryloxyphenoxypropionic acid herbicide in the glufosinate-aryloxyphenoxypropionic acid herbicide weeding composition is in a range of (50: 1) to (1: 1). The glufosinate-aryloxyphenoxypropionic acid herbicide weeding composition comprises 10 to 80wt% of glufosinate and the aryloxyphenoxypropionic acid herbicide. The glufosinate-aryloxyphenoxypropionic acid herbicide weeding composition can be used for preventing and removing weeds in bare places, orchards and field ridges, has effects superior to effects of a single aryloxyphenoxypropionic acid herbicide or glufosinate, reduces a use amount of a pesticide, reduces the adverse influence produced by a pesticide on the ecological environment, and effectively solves the problem of weed resistance to pesticides.

Methods for controlling a density of algae growing in an aquatic environment are provided. Exemplary methods include applying an effective amount of glyphosate to a density of algae growing in an aquatic environment. The algae may include genus Nannochloropsis and/or Dunaliella. The algae may also include a glyphosate resistant strain of genus Nannochloropsis. The effective amount may result in an approximate concentration of between 0.1 millimolar to 0.3 millimolar glyphosate in the aquatic environment. Additionally, the aquatic environment may include seawater. The glyphosate may be applied to the aquatic environment before and/or after the aquatic environment is inoculated with algae. Alternative methods include applying an effective amount of glufosinate to a density of algae growing in an aquatic environment.

The invention discloses a method used for synthesizing glufosinate and an analogue of glufosinate by taking methylphosphoric dichloride and 2-hydroxy butane-3-nitrile as initial raw materials. According to the method, esterification is carried out so as to obtain methyl phosphite ester (I) and 2-acetyloxy-3-butenenitrile (II), intermediate (3-acetyloxy-3-cyano-propyl)-methylphosphonate (III) is obtained via Michael free radical addition, and glufosinate and the analogue (IV) are obtained via ammoniation and hydrolysis. Synthetic route of the method is short; yield is high; by-product is less; product purity is high; and the method is suitable for industrialized production.

The invention provides a glufosinate purifying technology including the following steps: (1) adding glufosinate hydrochloride to alcohol R1OH, adding R2NH2 for ammoniation, adjusting the pH to 7.0-14.0, cooling and filtering, removing a solvent from a filtrate to obtain glufosinate ammonium salt and a small amount of organic impurities; (2) dissolving the glufosinate ammonium salt obtained by the steps (1) in an appropriate amount of water, leading in CO2 for neutralizing to the pH of 2.0-5.0, adding a proper amount of alcohol R3OH for precipitation of glufosinate acid, centrifugally filtrating to obtain the glufosinate acid which contains a small amount of ammonium hydrogen carbonate or organic amine carbonates; (3) heating for drying a glufosinate acid filtering cake obtained by the step (2) for decomposition and volatilization of the ammonium hydrogen carbonate or organic amine carbonates to obtain high purity glufosinate acid. The glufosinate purifying technology is simple in steps, the obtained glufosinate is low in inorganic salt content and high in purity, and compared with a traditional technology using epoxy ethane and epoxy propane, the purifying technology using carbon dioxide for separation of glufosinate hydrochloride and HCl is more economical, and high in safety, and has a higher industrialization prospect.

The invention belongs to the technical field of organic compound synthesis and relates to a preparation method of fine glufosinate, in particular to a preparation method of fine glufosinate with L-homoserine as a raw material. According to the preparation method of fine glufosinate, L-homoserine prepared through a biological fermentation method serves as an initial raw material, L-3,6-di(2-halogenethyl)-2,5-diketopiperazine is prepared through the steps such as azeotropic dehydration and halogenation, a Serhiy Arbuzov reaction is conducted between L-3,6-di(2-halogen ethyl)-2,5-diketopiperazine and methyl phosphonic acid dibutyl, and fine glufosinate is prepared through a hydrolysis reaction. Compared with an existing preparation technology, the preparation method of fine glufosinate has the advantages that the total yield of fine glufosinate is greatly increased, the technological process is simple, and fine glufosinate is suitable for industrial production.

The invention relates to a synthesizing method for pesticide glufosinate, i.e., ((D,L)-2-amino-4-(hydroxyl(methyl)phosphinyl)butyrate) and a salt of an acid or an alkali thereof. In the synthesizing method, the pesticide glufosinate is prepared by undergoing a strecker reaction, and an intermediate compound, i.e., (3-nitrile-3-hydroxy)propyl methyl phosphonic acid directly reacts with carbon dioxide and ammonia gas in an aqueous solution to synthesize the pesticide glufosinate and a salt of an acid or an alkali thereof. The method comprises the following specific steps of: adding the intermediate compound, i.e., (3-nitrile-3-hydroxy) propyl methyl phosphonic acid into a high-pressure kettle; adding carbon dioxide, ammonia gas and water, wherein ammonium bicarbonate or ammonium carbonate and the like can be used for replacing carbon dioxide carbon and ammonium, the molar ratio of the intermediate to the carbon dioxide is between 1 and 12, and the ratio of the ammonia gas to the carbon dioxide is between 0.5 and 5; adding 15-75 times of water; heating to 120-180 DEG C; reacting for about 4-20 hours; and after the reaction, cooling, taking the reaction liquid out, and concentrating to directly obtain an ammonium salt of glufosinate. The yield is over 80 percent.

The invention relates to a new preparation method for herbicide glufosinate. The method comprises the following steps of: performing Bucherer-Bergs cyclization reaction on a methylphosphonate derivative type compound (II), ammonium carbonate and cyanide serving as raw materials to obtain a compound shown by a formula (III); and then hydrolyzing to prepare glufosinate compound shown by a formula (I). According to the preparation method, hemiacetal or acetal is used as a raw material, and the Bucherer-Bergs cyclization reaction is performed to obtain a glycolylurea derivative, so that high yield, easiness for detection and mild condition are guaranteed; and after glycolylurea is cyclihydrolyzed, a product has high purity, and ammonium salt can be removed without multiple recrystallization processes.

The invention discloses a glufosinate-picolinic acid herbicide weeding composition. The glufosinate-picolinic acid herbicide weeding composition comprises glufosinate and a picolinic acid herbicide as active ingredients, and the balance pesticide assistants. A weight ratio of glufosinate to the picolinic acid herbicide in the glufosinate-picolinic acid herbicide weeding composition is in a range of (20: 1) to (1: 10). The glufosinate-picolinic acid herbicide weeding composition comprises 10 to 80wt% of glufosinate and the picolinic acid herbicide. The glufosinate-picolinic acid herbicide weeding composition can be used for preventing and removing weeds in bare places, orchards and farmlands, has effects superior to effects of a single picolinic acid herbicide or glufosinate, reduces a use amount of a pesticide, reduces the adverse influence produced by a pesticide on the ecological environment, and effectively solves the problem of weed resistance to pesticides.

The invention discloses a weeding composition with glufosinate and efficient haloxyfop methyl, and a preparation method of the weeding composition, and belongs to the agricultural field and aim to solve the problems that glufosinate has a poor prevention effect on perennial resistant plants, limitation of prevention and movement for perennial weeds, low weeding effect and high cost with exclusive use because of long-term massive use. The dosage form of the weeding composition is microemulsion and comprises glufosinate and efficient haloxyfop methyl. The ratio by weight of the glufosinate to efficient haloxyfop methyl is 1:5 to 45:1. The weeding composition prepared by the method has the characteristics of wide weeding range, high weeding effect and low cost. The pesticide effect is obviously better than any one of the glufosinate and the efficient haloxyfop methyl. The preparation method is simple and convenient to operate, and has the advantages of high feasibility, stable product quality and obvious market value. The composition still has good stability after being stored for a long time, thereby having obvious market values and being suitable for extensive generalization and use.

The invention provides a synthesis method for glufosinate shown as a formula (V) and an analogue thereof. The method comprises the following steps of: preparing an intermediate such as methyl diethyl phosphate by Grignard, disproportionation and coupling and with phosphorus trichloride, triethyl phosphate and chloromethane as initiative raw materials; condensing the methyl diethyl phosphate, anhydride and acrolein substances; performing Strecker reaction and hydrolysis and thus obtaining the glufosinate and the analogue thereof. In the synthesis method, the reaction condition is mild; safety is high; and yield is obviously increased.

The invention relates to a preparation method of glufosinate. The preparation method comprises the following steps: with a compound represented by a formula (I) as a starting material, reacting the compound represented by the formula (I) with cyanide RCN to obtain ketone nitrile; then hydrolyzing ketone nitrile in the presence of an acidic substance and water so as to obtain ketoacid; and reacting ketoacid successively with ammonia gas and hydrogen under the action of a catalyst so as to obtain glufosinate; wherein the compound represented by the formula (I) is cyclic phosphonic acid anhydride. The preparation method in the invention has the advantages of simple process, convenient operation, high product purity, high yield, no need for repeated recrystallization, ect.; and the final product of the preparation method is directly glufosinate ammonium, the step of converting glufosinate chloride into glufosinate ammonium is omitted, so the method has great economic benefit and is suitable for industrialization production.

The invention discloses a synergistic herbicidal composition for an uncultivated land and an orchard. The synergistic herbicidal composition consists of glufosinate and dicamba serving as active ingredients and acceptable auxiliary components in pesticides, wherein the weight ratio of the glufosinate to the dicamba is 1:3.2-10:1. After the two active ingredients are compounded, the synergistic herbicidal composition has the herbicide effect obviously superior to that of single glufosinate or single dicamba, has obvious synergism, can control perennial vines, undershrub weeds and broadleaf weeds and also can control annual and biennial weeds; and the herbicidal spectrum is enlarged, the use amount of single glufosinate and single dicamba is reduced, the production cost is reduced, and the herbicidal composition has obvious market popularization value.

The invention discloses a weedicide composition and a preparation method thereof, wherein the weedicide composition comprises the following components in percentage by weight: 1-50% of glyphosate and 0.1-50% of glufosinate-ammonium. The weedicide composition disclosed by the invention has the advantages that the glufosinate-ammonium can be compounded with the glyphosate, and the glufosinate-ammonium has no negative effect on the using effect of the glyphosate, so that the resistance problem of the single glufosinate is solved, the using cost of the glufosinate-ammonium is also effectively reduced, meanwhile, the weeding speed of the glufosinate is accelerated, and the using effect of a glufosinate product is also enhanced.