335 results about "Dichlorophenol" patented technology

The invention relates to a preparation method of herbicide dicamba. The preparation method includes: (1) liquid potassium hydroxide and 2, 5-dichlorophenol are reacted according to molar ratio of 0.95:1-1:1 to obtain 2, 5-dichlorophenol potassium; (2) at the presence of anhydrous potassium carbonate and catalyst, the 2, 5-dichlorophenol potassium obtained in the step (1) is reacted with CO2 to generate 3, 6-dichlorosalicylic acid, pressure of CO2 is controlled to be 4-6MPa, reaction temperature ranges from 100 DEG C to 160 DEG C, and molar ratio of anhydrous potassium carbonate and 2, 5-dichlorophenol potassium is 1-2:1; and (3) in alkaline condition, at the temperature of 70-100 DEG C, the 3, 6-dichlorosalicylic acid obtained in the step (2) and chloromethane are reacted under the action of the catalyst through a tube fixed-bed reactor according to molar ratio 1:1-3.5, saponification and acidification are performed to obtain 3, 6-dichloro-2-methoxysalicylic acid, namely the dicamba. The process is high in reaction yield, simple in reaction condition, good in product quality, small in three wastes and low in energy consumption.

The invention discloses a preparation method of 3,6-dichloro-2-hydroxybenzoic acid, which sequentially comprises the following steps: 1) salifying 2,5-dichlorophenol; 2) carboxylation: transferring the 2,5-dichlorophenate solution into a high-pressure reaction kettle, adding a cocatalyst, and introducing CO2 to carry out high-pressure carboxylation reaction to obtain the reaction product containing 3,6-dichloro-2-hydroxybenzoate, wherein the cocatalyst is composed of potassium carbonate and activated carbon; 3) refinement: after cooling the reaction product containing 3,6-dichloro-2-hydroxybenzoate obtained in the step 2) to room temperature, adding an alkali solution, regulating the pH value to 11-13, uniformly stirring, filtering to recover activated carbon, stratifying the filtrate, and taking the water phase; and adding an acid solution into the water phase, regulating the pH value to 1-3, carrying out vapor distillation to recover the 2,5-dichlorophenol, cooling to crystallize, carrying out vacuum filtration, and drying to obtain the 3,6-dichloro-2-hydroxybenzoic acid.

The invention relates to a method for preparing magnetic porous polystyrene microspheres on the basis of suspension polymerization, belonging to the technical field of preparation of environmental functional materials. The method comprises the following steps: synthesizing Fe3O4 magnetic particles by a solvothermal process; and preparing magnetic porous polystyrene microspheres by suspension polymerization by using styrene and divinylbenzene as functional monomers, azodiisobutyronitrile as an initiator and toluene and cyclohexanol as pore-forming agents. The obtained microspheres have abundant pores on the surface, thereby being beneficial to enhancing adsorbability; and the Fe3O4 magnetic particles inside the microspheres have magnetic stability, and can be quickly separated under the action of an external magnetic field. The adsorbent is used in a water environment for selectively adsorbing 2,4-dichlorophenol and 2,6-dichlorophenol. The static adsorption experiment result indicates that the magnetic porous microspheres prepared by the method have the advantages of favorable adsorption capacity, quick adsorption kinetic property and favorable regenerability.

The invention discloses a Pseudomonas aeruginosa strain TBPY, which is screened from tribromophenol(TBP)-polluted sludge and purified. The purified strain is domesticated by a pressure type domesticating method with gradually increased TBP concentration in an organic salt culture medium, and the domesticated strain can be used for the biological control of waste water containing persistent organic pollutants such as phenol, pyrocatechol, resorcinol, benzoic acid, p-hydroxybenzoic acid, vanillin, 4-chlorophenol, 2,4-dichlorophenol, trichlorophenol and tribromophenol and has high research and application values.

The invention relates to a carbon quantum dot and titanium codoped mesoporous silica composite photocatalyst and a preparation method thereof. The method is mainly characterized by comprising the following steps: simultaneously introducing carbon quantum dots and a titanium source in the process of synthesizing an ordered mesoporous silica material by using an in-site loading method, removing a template agent by using a solvent extraction method, and subjecting the carbon quantum dots to crystallization with the manner of calcination in an inert atmosphere so as to obtain the carbon quantum dot and titanium codoped composite photocatalyst. Compared with the prior art, the method provided by the invention has the following advantages: simplicity, convenience, easy operation, and highly-efficient utilization of raw materials are realized; meanwhile, the carbon quantum dots and the titanium can be codoped into pore walls of a mesoporous material, and synergistic effects are generated in the pore walls, so improvement of photocatalytic activity is promoted; meanwhile, ordered mesoporous channels also provide good channels for diffusion and transmission of guest molecules, so the prepared photocatalyst has good catalytic degradation activity to organic pollutants like acid orange 7 (AO7) and 2,4-dichlorophenol (2,4-DCP).

The invention discloses a method for removing 2,4-dichlorophenol in water by using polyurethane sponge fixed white rot fungi, belonging to the field of environmental microbiology. The method comprises the following steps: preprocessing a carrier, preparing fixed white rot fungi and removing 2, 4-dichlorophenol in water. The carrier has the characteristics of porosity, hydrophily and good adsorbability, enjoys stable chemical property and hydrolytic resistance, high organism bearing capacity and mass transfer rate and is not soluble in acid/alkaline water solution; while the fixed carrier can effectively absorb and fix white rot fungi, improve capacity of fixed white rot fungi in removing 2,4-dichlorophenol in water and leads the fixed white rot fungi to be easily separated from the product, thus being applicable to execute biological reaction processing on multiple sewages.

The invention provides a method of treating the phloroglucinol producing wastewater and the recycle utilization of the recovery organic compounds. The wastewater of the phloroglucinol producing with 2, 6-dichlorophenol and excess KOH as material is adjusted by hydrochloric acid to pH less than 3 before adsorbed by high-crosslinked adsorption resin. The secondary effluent water of adsorption is adjusted to be neutral by KOH before distilled. The KCl is recovered after the cooling crystallization and the centrifugal of the residue. The distilled effluent returns to the former manufacturing process to be indiscriminate used or biochemical treated by aerobic and discharges in standard. The distilled mother liquor merges into other batch of secondary effluent water of adsorption. The resin adsorbing the phloroglucinol is desorbed by KOH. The desorption liquid is applied in the hydrochloric acid acidization step of the former manufacturing process or hydrochloric acid is adopted directly to neutralize to be neutral before centrifugal separation to get phloroglucinol. By adopting the method, phloroglucinol and KCl can be recovered while the wastewater is treated. The pollution is reduced and the cost is saved. The organic combination of wastewater treatment and resource recovery as well as recycle utilization is realized.

The invention discloses a preparation process of chlorinated phenol; phenol is used as a raw material, a mixture of arbitrary one of diphenyl sulfide and dimethyl sulfide, arbitrary one of acetic acid and toluene sulfonic acid and arbitrary one of aluminum trichloride and ferric trichloride is used as a catalyst, a chlorinated phenol crude product is generated through sulfuryl chloride chlorination, and a target product is obtained by melt crystallization. The mixed catalyst used in the reaction has a positioning function, the content of p-chlorophenol in the monochlorophenol mixture generated from the reaction is greater than 83%, the content of 2,4-dichlorophenol in dichlorinated phenol generated from the reaction is greater than 98%, the amount of trichlorinated phenol impurities generated from the reaction is reduced, and 2,4,6-dichlorophenol with the content greater than 99% and the total yield more than or equal to 98% is obtained without purification treatment; moreover, energy consumption is greatly reduced, and high-content p-chlorophenol and high-quality 2,4-dichlorophenol can be produced at the same time.

The invention relates to a preparation method and application of a Mn-doped ZnS quantum dot imprinted sensor and belongs to the technical field of environmental functional material preparation. The method comprises the steps of firstly stirring an aqueous solution of zinc sulfate heptahydrate and an aqueous solution of manganese chloride tetrahydrate at room temperature under the condition that nitrogen gas is introduced, and adding an aqueous solution of sodium sulfide nonahydrate, so as to obtain Mn-ZnS quantum dots; carrying out vinyl modification on the obtained Mn-ZnS quantum dots by using 3-(methacryloyloxy) propyl trimethoxysilane, then, synthesizing a Mn-doped ZnS quantum dot imprinted sensor, which takes 2,6-dichlorophenol as template molecules, methacrylic acid as functional monomers, Mn-ZnS-KH570 as auxiliary monomers, ethylene glycol di(methacrylate) as a cross-linking agent, 2,2-azodiisobutyronitrile as an initiator and acetonitrile as a solvent, by using a precipitation polymerization method through two-stage polymerization, and applying the Mn-doped ZnS quantum dot imprinted sensor to the optical detection on 2,6-dichlorophenol. The prepared phosphorescent molecular-imprinted polymer has very good optical and pH stability and has the capability of selectively identifying 2,6-dichlorophenol.

The invention provides a method for synthesizing TiO2 composite photocatalyst with high selectivity and degradation function, belongs to the technical field of new material synthesis, and solves the problem of low selectivity in the prior photocatalysis reaction. The method for synthesizing the TiO2 composite photocatalyst with the high selectivity and the degradation function comprises the following steps: a, preparing titanium dioxide colloidal sol; b, performing hydrolytic condensation; and c, preparing the TiO2 composite photocatalyst. The TiO2 composite photocatalyst synthesized by the method for synthesizing the TiO2 composite photocatalyst with the high selectivity and the degradation function has high selectivity; and the method has the advantages of quick degradation and high degradation efficiency for 2, 4-dichlorophenol, and the like.

The invention provides a preparation method of 2,5-dichlorophenol, and belongs to the field of preparation of compounds. The preparation method comprises the following steps: taking 1,4-dichlorobenzene as a raw material and taking a combination of one or more of water, methanol, acetonitrile and acetic acid as a solvent under the effects of an oxidizing agent, a metal porphyrin catalyst and a cocatalyst, and reacting at the temperature of 5-80 DEG C for 0.5-20 hours to obtain 2,5-dichlorophenol. By a catalyst system, efficiency and yield of oxidation reaction can be improved remarkably, reaction conditions are gentle relatively, side effects are less, products are separated favorably, the reaction time is greatly shortened, and the 2,5-dichlorophenol can be industrially produced on a large scale.

The present invention relates to an improved preparation method for synthesizing phloroglucin. Said invention uses 2.4-dichlorophenol or 2.6-dichlorophenol as original raw material, and utilizes potassium hydroxide and inert solvent with high boiling point to make reaction of first-elimination after-addition to prepare phloroglucin by means of one-step process. Its yield is 56.6%-65.2%.

The invention provides an application of a calcium-manganese oxide catalyst in degradation of organic pollutants in wastewater and soil, and relates to the technical field of catalysis and environmental organic pollutant control. The calcium-manganese oxide (Cax(Mn1-aFea)yOz) catalyst is prepared by a sol-gel method and high-temperature calcination, and is used for activating persulfate to generate active substances with strong oxidizing property, such as sulfate free radicals, hydroxyl free radicals, singlet oxygen and the like, so that organic pollutants in water and soil are rapidly oxidized and removed. The catalyst disclosed by the invention is simple to prepare and environment-friendly, the contained elements are Ca and Mn elements which are low in toxicity, cheap and rich in the earth, the metal dissolution rate in the reaction process is low, and the problem of secondary pollution is avoided. In addition, the reaction system formed by the catalyst and persulfate can rapidly degrade phenol, bisphenol A, 2,6-dichlorophenol, parachlorophenol, paracetamol and other refractory organic pollutants, shows good performance in a wide pH range, and has great application potential.

The invention discloses a preparation process of 2,4-dichlorophenol. The preparation process comprises the following steps: chloridizing phenol or o-chlorophenol serving as a raw material and a mixture which is prepared from boric acid, phenyl sulfide and ferric trichloride and serves as a catalyst to generate a 2,4-dichlorophen coarse product, and rectifying the coarse product to obtain a target product. The mixed catalyst used in the reaction has a positioning effect, so that the content of p-chlorophenol in a chlorinated phenols mixture generated by the reaction is greater than 65 percent, the content of the 2,4-dichlorophenol in di-chlorophenol generated in the reaction is greater than 95 percent, the number of di-chlorophenol impurities generated in the reaction is reduced, and the 2,4-dichlorophenol with the content greater than 99.5 percent and the total yield of 95 percent or above can be obtained by rectification treatment; furthermore, the reaction yield is greatly increased, and the yield of the p-chlorophenol is also increased.

The invention discloses a synthetic method for 3,6-dichloro-2-hydroxybenzoic acid, which sequentially comprises the following steps: 1) salifying 2,5-dichlorophenol, 2) performing carboxylation, and 3) performing refinement, wherein according to Step 2), a 2,5-dichlorophenol saline solution is transferred into a high-pressure reactor, a catalyst is added, CO2 is supplied for high-pressure carboxylation reaction, a reaction product containing 3,6-dichloro-2-hydroxybenzoic acid salt is obtained, and the catalyst is potassium chloride; and according to Step 3), an alkaline solution is added after the reaction product is cooled to a room temperature, pH is adjusted to 11-13, an aqueous phase is obtained after layering, an acid solution is added to the aqueous phase, the pH is adjusted to 1-3, and after vapor distillation is performed and 2,5-dichlorophenol is recovered, suction filtration and drying are performed, and 3,6-dichloro-2-hydroxybenzoic acid is obtained. 3,6-dichloro-2-hydroxybenzoic acid synthesized with the method has the characteristics of low cost and higher yield.

The invention discloses an improved preparation method of 3,6-dichloro salicylic acid. The improved preparation method of 3,6-dichloro salicylic acid comprises the following steps: carrying out reaction on 2,5-dichlorophenol and an alkali liquor, then adding an organic solvent, and carrying out reduced pressure dehydration; adding potassium carbonate, a dehydrating agent and a stabilizer after dehydration is finished, and carrying out reaction at the temperature of 130-140 DEG C for 30-60 minutes; adding materials into a high pressure autoclave, heating to 130-140 DEG C, then introducing CO2, and carrying out high pressure carboxylation reaction; carrying out aftertreatment after the reaction is finished, so that 3,6-dichloro salicylic acid is obtained. The improved preparation method of 3,6-dichloro salicylic acid has the advantages that oxygen is isolated before dehydration and carboxylation, so that oxidation of oxygen to a product is avoided; the dehydrating agent and the stabilizer are added before carboxylation, so that water in a system and positive hydrogen ions generated during carboxylation are further removed, stability of the system is maintained, yield is guaranteed and appearance of the product is greatly improved, usage amount of potassium carbonate is reduced, and an aftertreatment process is simplified; besides, modification on equipment is less, the current production enterprises can implement improvement conveniently, and quick benefit can be obtained.

The invention relates to a process for preparing 2,4-dichlorphenoxyacetic acid with high quality; and the process comprises the following steps of: using phenol as a raw material; first chlorinating the phenol so as to prepare 2-chlorophenol, 4-chlorophenol and 2,4-chlorophenol; separating out the 2-chlorophenol through rectifying; further chlorinating the 4-chlorophenol to obtain 2,4-dichlorophenol immediate with mass percentage of not less than 98%; and under an alkaline condition, reacting the 2,4-dichlorophenol immediate with chloroacetic acid, so as to obtain 2,4-dichlorphenoxyacetic acid with mass percentage of not less than 98%. Compared with the prior art, the process for preparing 2,4-dichlorphenoxyacetic acid with the high quality, provided by the invention, has the advantages as follows: the 2,4-dichlorphenoxyacetic acid (98%) with high quality is obtained; meanwhile, untransformed 2,4-dichlorophenol is recycled through solvent extraction and is recycled as reaction raw material for the next reaction through being neutralized and alkalified; therefore, the environment friendly process for preparing the 2,4-dichlorphenoxyacetic acid with high quality and high yield is provided.