57 results about "Dichloroprop" patented technology

The invention discloses a preparation method of phosphorus and nitrogen contained acrylate and copolymer core-shell particles of the phosphorus and nitrogen contained acrylate. Phenylphosphonic dichloride, hydroxyethyl acrylate and diethylamine which are taken as raw materials react with trimethylamine as an acid binding agent in tetrahydrofuran at 0-5 DEG C, and phosphorus and nitrogen contained acrylate is prepared. The synthesis method is simple, and the cost is low. The phosphorus and nitrogen contained acrylate can be subjected to free-radical copolymerization with other acrylate monomers. The core-shell particles of the phosphorus and nitrogen contained acrylate are prepared with a core-shell emulsion polymerization method, the core-shell particles have the advantages of adjustable structure and composition, have certain flame retardancy on the premise that the structure of a core-shell impact modifier is not changed and are expected to be used for toughening flame retardant materials.

The invention provides a method for treating byproducts in a process for preparing chloropropene by propylene chlorination. The method comprises the following steps: separating byproducts in a processof preparing chloropropene by propylene chlorination to obtain cis-1, 3, 5-triazolo[1, 2-a]pyridin-2-carboxylic acid. According to the method, trans-1, 3-dichloropropene reacts and is converted intotrans-1, 3-dichloropropene with higher additional value under the illumination condition and the catalytic action of the catalyst, so that the economic value of byproducts in the process of preparingchloropropene by propylene chlorination is improved, the cost of the whole process is greatly reduced, and the method has a good industrial application prospect.

The invention relates to a high-efficiency soil disinfection and activation technology for preventing and controlling protected vegetable soil-borne diseases. The technology comprises the following operation steps: in a leisure period after harvest of preceding crops in summer and autumn, cleaning fields, performing fertilization and rotary tillage, and then performing field irrigation; when the water content of soil reaches about 60-70%, spraying lime nitrogen granules; performing rotary tillage and soil mixing on the soil; applying 1,3-dichloropropene emulsion oil; performing seal by coverage with plastic film for 20-30 days, then uncovering the film for airing for 7-10 days, completing fumigation disinfection on soil; applying biological bacterial fertilizer to the field after the fumigation disinfection; performing ecological restoration and activation on the soil, so as to establish beneficial microbial flora of the soil. The technology provided by the invention is mainly used forpreventing and controlling the protected vegetable soil-borne diseases caused by pathogenic nematodes, fungi and bacteria. The technology has a notable effect and a long lasting period of preventingand controlling the soil-borne diseases, has a promoting effect on the crop growth, and particularly has a notable effect of root-knot nematode prevention. The soil disinfection technology is economicand high efficient, and has low cost and notable benefits.

The invention discloses a herbicidal compositions containing safety agent, which contains 3-methyl-2-[5-(2-chlor-4- trifluoromethylphenoxy)-2-nitrylbenzoxy]-3-ethyl crotonate(SYP-249) as effective constituent and a herbicidal safety agent selected from fenchlorazole, mefenpyr-diethyl, dichlormid, brassinolide. Herbicidal compositions is respectively processed to missible oil, suspending agent (emulsion), aqueous emulsion, microemulsion, water dispersed granule, wettable powder. Disposal of the wheat leaf and growth spot with the said composition can relieve the damage to wheat of herbicide without influencing the weeds prevention and expelling effect.

Less colored trans-1,3-dichloropropene and a process for producing it, are presented.A composition comprising cis-1,3-dichloropropene, trans-1,3-dichloropropene and C6 compounds, is subjected to a distillation step and to a step of reacting chlorine or bromine, to remove cis-1,3-dichloropropene as a low boiling component, and then the residue is distilled to remove the chlorinated C6 compounds as a high boiling component and to obtain trans-1,3-dichloropropene as a low boiling component.

The invention relates to wettable powder, powder or a microgranule preparation prepared from accessory ingredients, such as a wetting agent, a dispersing agent, fillers and the like, and a pesticide composition containing dazomet and 1,3-dichloropropylene for controlling soil-borne diseases such as Phytoph-thora capsici Leonian and the like as well as Meloidogyne. The invention also discloses a method for preventing the soil-borne diseases such as the Phytoph-thora capsici Leonian and the like as well as Meloidogyne by using the composition containing the dazomet and the 1,3-dichloropropylene. The dazomet and the 1,3-dichloropropylene are mixed at the ratio of (1:2)-(2:1) to especially perform action on the Phytoph-thora capsici Leonian and the Meloidogyne. The pesticide composition is not only used for controlling the Phytoph-thora capsici Leonian and the Meloidogyne, but also widely applied to the aspects of controlling the soil-borne diseases (including the meloidogyne) in vegetables, such as hot peppers, gingers, cucumbers and the like, field crops and flowers. The pesticide composition has high application value and obvious economic and social benefits.

The invention relates to a preparation method and an application method of a pyrazole oxime derivative (I) containing dichloropropene. The pyrazole oxime derivative is obtained by condensing pyrazole hydroxyl oxime (II) and a terminated bromo compound (III) containing dichloropropene. The pyrazole oxime derivative containing dichloropropene has an effective effect of preventing and controlling harmful insects, and the pyrazole oxime derivative can be used for preparing insecticides in such fields as agriculture and horticulture (As shown in Specification).

The invention discloses a method for detecting residual quantity of dibromochloropropane and 1, 3-dichloropropene in vegetables and fruits by gas chromatography-mass spectrometry. The method comprisesthe following steps: pretreatment, headspace (HS) sample introduction, GC-MS / MS (Gas Chromatography-Mass Spectrometry-Mass Spectrometry) determination and quantification by an external standard method. According to the method, the detection limit of dibromochloropropane is as low as 0.4 mu g / kg, the recovery rate is 87.08%-104.86%, and the RSD value is 5.28%-8.29%; the detection limit of 1, 3-dichloropropene is as low as 2 mu g / kg, the recovery rates of cis / trans isomers are 88.82%-119.45% and 87.20%-116.55% respectively, and the RSD values are 3.49%-8.14% and 1.15%-9.72% respectively. The method is easy to operate, environment-friendly, high in sensitivity and good in reproducibility.

The invention belongs to the technical field of chemical industry, and discloses a trans-1, 3-dichloropropene compound, a cis-1, 3-dichloropropene compound, a cis-trans-1, 3-dichloropropene compound and a rectification method thereof, the dichloropropene compound is composed of the trans-1, 3-dichloropropene and the cis-1, 3-dichloropropene or the cis-trans-1, 3-dichloropropene; the trans-1, 3-dichloropropene is mainly used for preparing chloramine, and the chloramine is used for preparing final product clethodim. The cis-trans mixed 1, 3-dichloropropene is used as a soil fumigant and a soil insecticide, radically treats underground nematodes and replaces methyl bromide in a methyl bromide project of the United Nations. The cis 1, 3-dichloropropene and a cis-trans mixed 1, 3-dichloropropene product are blended to serve as the cis-trans mixed 1, 3-dichloropropene to be still used for radically treating the underground nematodes. The dichloropropene compound can inhibit or directly killvarious nematodes and relieve nematode disease damage, the control effect reaches 98% or above, and the lasting period is 3 months or above.

The present invention relates to a method capable of utilizing DD mixture to prepare acrylate and separating 1,2-dichloropropane from it. Said invention utilizes the action of 1,3-dichloropropene in the DD mixture and acrylic acid or methylacrylic acid, alkali, catalyst and and polymerization inhibitor to synthesize 3-chloro-2-propenyl acrylate or 3-chloro-2-propenyl 2-methacrylate, and utilizes the distillation to make it be separated from 1,2-dichloropropane. Said method includes the steps of raw material pretreatment, catalytic esterification reaction, product separation and product refinement.

The invention discloses a method and a system for producing 1, 3-propylene glycol by a multi-step method. The method comprises the following steps: carrying out dehydration reaction on 1, 3-dichloropropanol and a dehydration catalyst to prepare 1, 3-dichloropropene; carrying out a first hydrolysis reaction on a first mixed reaction system containing the 1, 3-dichloropropene, a first hydrolysis agent and a first solvent to prepare 3-chloro-2-propene-1-alcohol; carrying out hydrogenation reaction on the 3-chloro-2-propene-1-alcohol and a hydrogenation catalyst to prepare 3-chloropropanol; and carrying out a second hydrolysis reaction on a second mixed reaction system containing the 3-chloropropanol, a second hydrolysis agent and a second solvent to prepare the 1, 3-propylene glycol. According to the method, 1, 3-dichloropropanol is used as a raw material, the important chemical raw material 1, 3-propylene glycol is prepared through a dehydration, hydrolysis, hydrogenation and hydrolysisfour-step method, and the method has the advantages of mild reaction conditions, low cost, environmental protection, economy and the like.

The invention provides a production method of cis or trans-1, 3-dichloropropene, mutual conversion of cis or trans-1, 3-dichloropropene can be carried out under the condition that visible light or ultraviolet light is not needed by using a catalyst, the conversion direction can be freely selected according to actual requirements, the equipment is simple, the cost is low, and the production method is suitable for industrial production. According to the technical scheme of the invention, the catalyst is simple in preparation process and free of special design, the same set of equipment can be used for preparing trans-1, 3-dichloropropene from cis-1, 3-dichloropropene and can also be reversely operated, only corresponding products need to be controlled to enter the product tank and the raw material tank by using pipelines, and the catalyst in the technical scheme of the invention is low in price and easy to obtain, and can be used for preparing trans-1, 3-dichloropropene from cis-1, 3-dichloropropene. Various catalysts can be mixed without affecting the catalytic effect and can be obtained by recycling waste materials, the reactor does not need illumination, can be freely designed and can adapt to the large-scale production requirement, the gas phase of the reactor enters the rectifying tower through flash evaporation, continuous production can be achieved, and operation is easy and convenient.

The invention relates to a clean and environment-friendly production process of 2-chloro-5-chloromethylthiazole, which comprises the following steps: dissolving sodium thiocyanate in water, dropwiselyadding 2, 3-dichloropropene, carrying out heat preservation reaction after the dropwisely adding is completed, washing the obtained material with water, layering, and distilling to obtain an intermediate product 2-chloropropenyl isothiocyanate; dissolving the intermediate product in dichloroethane, dropwise adding sulfonyl chloride for the first time at the temperature of 30-60 DEG C, carrying out heat preservation reaction after dropwise adding is finished, degassing, desolventizing and cooling the obtained material, dropwise adding sulfonyl chloride for the second time, carrying out heat preservation reaction after dropwise adding for the second time, adding a stabilizer into the obtained material, and distilling to obtain 2-chloro-5-chloromethylthiazole. According to the invention, a pure byproduct sodium chloride is obtained, and the problem of high ammonia-nitrogen wastewater is solved. Due to the fact that the sulfonyl chloride is appropriate in use amount and is added in two times, by-products of sulfur dioxide and hydrogen chloride gas are reduced, the problem of environmental pollution is solved, and the production process is mild in reaction condition, small in toxicity,high in yield and purity and environmentally friendly.

The invention discloses a preparation method and application of a 1, 3-dichloropropene solid slow-release preparation. The preparation process is specifically as follows: the slow-release preparation is prepared by using an adsorption method of separation, that is, an absorbent carrier which has high absorption performance and desorption performance is adopted and used for absorbing the gasified 1,3-dichloropropene for 3 to 4 hours, thus obtaining different soil sanitizers with the content of 1,3-dichloropropene ranging from 5 to 40wt%, wherein the absorbent carrier comprises at least one of activated carbon, activated clay and a polymeric absorbent, and preferably, the absorbent carrier is the activated carbon; and the grain weight of the absorbent carrier is 0.5 to 10g. By adopting the product prepared by the method disclosed by the invention, the control effect the same as that of the stock solution can be gained, and the product is even wider in broad spectrum; specific experimental conditions can be saved; and the operation process is simple, the repeatability is great, and the effect of the soil sanitizer can be efficiently realized along with high quality. The method is wide in applicable scope and application prospect.

The invention provides a preparation method of trans-1, 3-dichloropropene, the preparation method adopts a specific catalyst to convert cis-1, 3-dichloropropene into trans-1, 3-dichloropropene, only needs the catalyst and illumination, does not need to add other solvents and assistants, and has the advantages of mild reaction conditions, simple process and easy industrial implementation. Few byproducts are produced in the reaction process, the subsequent separation is simple, and the application prospect is wide.

The invention discloses an anthranilic diamide compound containing dichloropropene based on a pyrazolone ring and synthesis and application thereof. The structure of the anthranilic diamide compound is shown in the general formula I shown in the specification. The compound is very effective for lepidoptera pests such as plutella xylostella and oriental armyworms and can be used for preparing insecticide in the fields of agriculture and gardening.

The invention discloses a preparation method of dichloropentachloromethylthiazole, which is characterized in that 2, 3-dichloropropene, sodium thiocyanate, sulfuryl chloride and the like are used as main raw materials, 2-chloro-5-chloromethylthiazole is prepared by changing a reaction solvent, reaction temperature and the like, and the product is purified. According to the preparation method of dichloropentachloromethylthiazole, 2, 3-dichloropropene, ammonium thiocyanate, sulfuryl chloride and the like are used as main raw materials, 2-chloro-5-chloromethylthiazole is prepared by changing a reaction solvent, reaction temperature and the like, and the product is purified. Experimental results show that dichloroethane is used as a solvent, 2, 3-dichloropropene and ammonium thiocyanate are sequentially subjected to a substitution reaction, an isomerization reaction and a chlorination-cyclization reaction through a one-pot process, the 2-chloro-5-chloromethylthiazole can be prepared through simple distillation, the purity can reach 99% or above, and the method is easy to operate, few in side reaction, few in three wastes and high in efficiency.

The invention discloses a pesticide composition and application thereof. Active components of the pesticide composition comprise 1,3-dichloropropene, dimethyl disulfide and trichloronitromethane. The composition disclosed by the invention is applicable to soil disinfection before planting for crops fields of vegetables, strawberries, flowers, melons, nursery gardens, orchards, tea gardens, forests, Chinese herbal medicines and the like, and can be used for effectively preventing and treating root-knot nematodes, soil-borne fungal pathogens, soil-borne pathogen bacteria and common weeds of farmlands, particularly heterodera glycines ichinohe, fusarium and digitaria sanguinalis, which commonly appear in a planting process of agricultural crops. The pesticide composition disclosed by the invention has an unexpected synergistic effect in a certain ratio range; the nematode killing, sterilization and weeding effects of the composition are obviously improved as compared with those of a single agent; meanwhile, the utilization dosage of pesticides, the pesticide application labor and the cost are reduced; and bad influences on the environment and pesticide residues are also reduced.

The present invention is a chemical synthesis method, a production method of the allyl dichloride amine. The technical proposal uses the two-step reaction; in the first step, the ammonia and the 3-allyl chloride react with the influence of the amine catalyst and the vinyl inhibitor to get the diallyl amine; in the second step, the diallyl amine and the dichloroacetyl chloride react to get the allyl dichloride amine. The allyl dichloride amine produced in the method has the advantages of the high content of the product, the little three-waste, the high production safety, the short production cycle and so on.

The invention belongs to the technical field of organic synthesis, and relates to a preparation method of trans-3-chloro-2-propenyl hydroxylamine for producing clethodim technical intermediates and other pesticide important intermediates, which specifically comprises the following steps: hydrolyzing trans-1, 3-dichloropropene serving as a raw material to obtain 3-chloropropenol; and reacting the obtained 3-chloropropenol with hydroxylamine salt under the catalysis of an acidic catalyst to generate the trans-3-chloro-2-propenyl hydroxylamine. By adopting the technical scheme, the preparation method disclosed by the invention has the beneficial effects that the raw materials are easy to purchase, the operation is simple and convenient, the yield is high, no pollution is caused, and industrial production is easy.

The invention provides a synergistic herbicidal composition comprising flucarbazone and diflufenican. The herbicidal composition includes the following active components: (A) flucarbazone and diflufenican, and (B) one or more selected from dimethenamid, dimethenamid-p, flupoxam, bicyclopyrone, 2,4-dichlorprop and a salt thereof, and 2,4-dichloroprop-p and a salt thereof, and additives being available in pesticide preparation processing. The herbicidal composition is processed to obtain a common herbicide preparation which is used for preventing and controlling undesirable plants.

The invention belongs to the technical field of organic synthesis, and particularly discloses a synthesis method of O-(3-chloro-2-propenyl) hydroxylamine. The synthesis method comprises the following steps of: carrying out a heating reaction on a hydroxylamine solution and methyl isobutyl ketone to obtain methyl isobutyl ketoxime, then carrying out a reaction on the methyl isobutyl ketoxime, 1, 3-dichloropropene and an alkali liquor, after the reaction is finished, adjusting the reaction liquid to be weakly acidic by using acid, carrying out phase splitting, extracting a water phase by using methyl isobutyl ketone, combining organic phases, washing with water, removing water, and recovering the methyl isobutyl ketone to obtain the product 0-(3-chloro-2-propenyl) hydroxylamine. According to the method, methyl isobutyl ketone serves as an amino protective agent and a solvent at the same time, the molecular structure is not changed before and after the reaction, the defects that a large amount of ethyl acetate is consumed and acetic acid and sodium chloride are produced as byproducts in a traditional process can be overcome, and the method is an efficient, environment-friendly and high-yield 0-(3-chloro-2-propenyl) hydroxylamine synthesis method and is suitable for industrial production.

The invention discloses a detection method of trans-1,3-dichloropropene in E-1-chloro-6, 6-dimethyl-2-heptenyl-4-yne. The detection method comprises the steps that the acceptable limit of trans-1,3-dichloropropene in (E)-1-chloro-6, 6-dimethyl-2-heptenyl-4-yne is determined to be less than or equal to 6 ppm, (E)-1-chloro-6, 6-dimethyl-2-heptenyl-4-yne is subjected to direct sample injection afterbeing dissolved by a solvent, and impurities, namely trans-1,3-dichloropropene, in (E)-1-chloro-6, 6-dimethyl-2-heptenyl-4-yne is subjected to qualitative and quantitative treatment through a GC-ECD detection method. Experiments show that the detection method has the advantages of easy operation, good specificity, sensitivity, accuracy and the like, the impurities, namely trans-1,3-dichloropropene, in (E)-1-chloro-6, 6-dimethyl-2-heptenyl-4-yne can be reliably subjected to qualitative and quantitative analysis according to the control requirements of genotoxic impurities.

The invention belongs to the technical field of production of compounds, and discloses a production method of a 2,3-dichloro-1-propene compound and a production device of the production method of the2,3-dichloro-1-propene compound. Liquid caustic soda and a catalyst are added into 1,2,3-trichloropropane, under a heating condition, the 1,2,3-trichloropropane is transformed into 2,3-dichloro-1-propene with a content higher than 90%, and the 2,3-dichloro-1-propene with the content higher than 90% is subjected to continuous rectification or batch rectification to produce 2,3-dichloro-1-propene with a content higher than 99%. A product produced through the production method of the 2,3-dichloro-1-propene compound and the production device of the production method of the 2,3-dichloro-1-propene compound is good in quality, high in yield and low in cost, therefore, the route method for producing the 2,3-dichloro-1-propene by means of the 1,2,3-trichloropropane, the liquid caustic soda and thecatalyst under the heating condition is suitable for large-scale popularization, a 2,3-dichloro-1-propene crude product can be obtained, the yield is higher than 98%, and the 2,3-dichloro-1-propene crude product is subjected to continuous rectification or batch rectification to produce 2,3-dichloro-1-propene with a content up to 99.8% or above.

The invention relates to a 1, 1-dichloropropene ether compound (I) containing N-substituent-3-methylpyrazole oxime unit structure, a preparation method and application thereof. The compound is obtained by reacting N-substituent-3-methylpyrazole oxime (III) with 3-(2, 6-dichloro-4-(3, 3-dichloro-4-(3, 3-dichloro allyloxy)phenoxy)-1-bromoalkane key intermediate (II). The 1, 1-dichloropropene ether compound (I) containing N-substituent-3-methylpyrazole oxime unit structure shows good control effect on harmful insects, and the compound can be used for preparing insecticides of agriculture, gardening and other fields. (general formula I).

The invention discloses a preparation method of fipronil derivative HNPC-A 8088, comprising: under the action of an organic solvent methanol, ethanol, n-propanol or butanone, and an inorganic alkali KOH, NaOH, Na2CO3 or K2CO3, reacting fipronil with trans-1,3-dichlorpropylene, and after reacting, performing filtering, desolventizing, filtering and recrystallizing to obtain the finished fipronil derivative HNPC-A 8088 >95% in mass content, having a following chemical reaction formula. A low-boiling-point organic matter is used as a reaction solvent so that product desolventizing temperature is reduced, the solvent is easy to recycle, reaction conditions are mild, operation is safe, product yield is greatly increased, a post-treatment method has simple process and low three wastes, saves energy and reduces consumption, and solved are the problems: the prior art is low in yield and high in cost, the organic solvent for use has a high boiling point, the product HNPC-A 8008 thermally decomposes easily if rectification desolventizing temperature is high, and there is a need for column chromatography to obtain a product while column chromatography is high in cost, low in capacity and difficult to industrialize.

A process is described for producing 2-chloroallyl isothiocyanate from 2,3-dichloro-1-propene by reacting the 2,3-dichloro-1-propene with a thiocyanate in the presence of a phase transfer catalyst, without diluent or in the presence of up to 15 percent by weight based on 2,3-dichloropropene and simultaneously in the presence of an excess of from 10 to 200 mol percent of 2,3-dichloro-1-propene based on the thiocyanate. A process starting from 1,2,3-trichloropropane is also described.

The invention discloses a method for obtaining cis-1,3-dichloropropene by in-situ inversion of trans-1,3-dichloropropene, which comprises the following steps: (1) preparing trans-1,3-dichloropropene as The raw material is to add trans-1,3-dichloropropene into an alcohol solvent to form an alcohol solution; (2) add a photoaccelerator to the alcohol solution; (3) irradiate the alcohol solution after adding the photoaccelerator to ultraviolet light , control the reaction temperature, and obtain cis-1,3 dichloropropene after the reaction. The conversion of trans-1,3-dichloropropene into cis-type 1,3-dichloropropene by the method of the invention has the advantages of low cost, environmental protection and high commercial value.

The invention belongs to the field of organic synthesis, and relates to a preparation method of chloramine, which comprises the following steps: reacting hydroxylamine salt, carboxylic acid ester and an acid-binding agent in a continuous flow reactor to obtain an intermediate product A; mixing the intermediate product A with a catalyst to obtain a mixture B, and reacting the mixture B with 1, 3-dichloropropene in a continuous flow reactor to obtain an intermediate product C; reacting the intermediate product C with hydrochloric acid in a continuous flow reactor to obtain an intermediate product D; uniformly mixing dichloromethane and the intermediate product D, and extracting to obtain an oil phase E and a water phase F; reacting the F with alkali in a continuous flow reactor to obtain an intermediate product H; uniformly mixing dichloromethane and the intermediate product H, and extracting to obtain an oil phase I and a water phase J; and I, performing continuous distillation by using a continuous distillation device, and continuously applying the recovered dichloromethane to obtain chloramine. The yield and the purity of the product are improved, the safety coefficient is increased, the cost is reduced, and the method is suitable for industrial production.