123results about "Preparation from carboxylic acid halide" patented technology

This invention provides a novel compound which can be properly used as a surfactant, a method of producing a fluoropolymer, surfactant and a fluoropolymer aqueous dispersions using the novel compound. This invention is a fluoroalkylcarboxylic acid derivative which is represented by the general formula (i): Rf1(OCH2CF2CF2)n1OCX1X2CF2(Rf2)n2COOM   (i) wherein Rf1 represents a straight or branched fluoroalkyl group containing 1 to 20 carbon atoms, which fluoroalkyl group may optionally contain 1 to 5 oxygen atoms in the principal chain thereof, Rf2 represents a straight or branched fluoroalkylene group containing 1 to 25 carbon atoms, said fluoroalkylene group may optionally contain 1 to 5 oxygen atoms in the principal chain thereof, n1 represents an integer of 0 to 3, n2 represents an integer of 0 or 1, X1 and X2 are the same or different and each represents hydrogen atom or fluorine atom, and M represents NH4 or a monovalent metal element.

This invention provides a novel compound which can be properly used as a surfactant, a method of producing a fluoropolymer, surfactant and a fluoropolymer aqueous dispersions using the novel compound.This invention is a fluoroalkylcarboxylic acid derivative which is represented by the general formula (i):Rf1(OCH2CF2CF2)n1OCX1X2CF2(Rf2)n2COOM  (i)wherein Rf1 represents a straight or branched fluoroalkyl group containing 1 to 20 carbon atoms, which fluoroalkyl group may optionally contain 1 to 5 oxygen atoms in the principal chain thereof, Rf2 represents a straight or branched fluoroalkylene group containing 1 to 25 carbon atoms, said fluoroalkylene group may optionally contain 1 to 5 oxygen atoms in the principal chain thereof, n1 represents an integer of 0 to 3, n2 represents an integer of 0 or 1, X1 and X2 are the same or different and each represents hydrogen atom or fluorine atom, and M represents NH4 or a monovalent metal element.

The invention discloses a preparation method of a fluoro-ether carboxylic acid surfactant. A fluorine-containing olefin monomer, oxygen and a molecular weight regulator are initiated to carry out the photochemical reaction by ultraviolet light to generate fluoro-ether acyl chloride and fluoro-ether acyl fluoride at the temperature of -40 to -80 DEG C, fluoro-ether acyl chloride and fluoro-ether acyl fluoride are hydrolyzed under the radiation of ultraviolet light to generate fluoro-ether carboxylic acid, and the fluoro-ether carboxylic acid is washed and purified to obtain a fluoro-ether carboxylic acid finished product. Through the adoption of the preparation method, the completely nontoxic fluoro-ether carboxylic acid surfactant can be produced, and can serve as a dispersing agent to completely replace perfluoro caprylic acid during the fluorine-containing polymer production process.

The invention relates to a method for preparing difluoroacetic acid and the salts thereof. The invention also relates to the preparation of difluoroacetyl fluoride used as an intermediate product in the preparation of difluoroacetic acid. The method for preparing difluoroacetic acid according to the invention is characterised in that the same comprises the step of preparing difluoroacetyl fluoride by reacting dichloroacetyl chloride with hydrofluoric acid in a gaseous phase and in the presence of a chromium-based catalyst, followed by the step of hydrolysing the difluoroacetyl fluoride thus obtained.

The invention relates to the technical field of fluorochemical preparation, particularly a preparation method of perfluoroheptanoic acid. The method comprises the following steps: oxidizing dodecafluoroheptanol to obtain dodecafluoroheptanoic acid, carrying out reaction on the dodecafluoroheptanoic acid and thionyl chloride to obtain dodecafluoroheptanoyl chloride, carrying out fluorination on the dodecafluoroheptanoyl chloride to obtain perfluoroheptanoyl chloride, and hydrolyzing to obtain the perfluoroheptanoic acid. The technical process of preparing perfluoroheptanoic acid from dodecafluoroheptanol has the advantages of low energy consumption, no pollution and high yield (up to 75% or above), is easy to operate, and has higher competitive edges than the existing perfluoroheptanoic acid production technique.

In the production of carboxylic acid or carboxylic acid ester, a reaction product containing the carboxylic acid or carboxylic acid ester which has been produced by the reaction of an olefin, carbon monoxide, and water or an alcohol in the presence of HF is heat-treated in the presence of an acid catalyst and an acid adsorbent. By the heat treatment, the contamination of the carboxylic acid or carboxylic acid ester with HF and / or fluorine compounds such as acyl fluorides can be prevented, to enable the stable production of a high quality and high purity carboxylic acid or carboxylic acid ester without causing troubles such as corrosion of apparatus.

The invention relates to a method for preparing bromodifluoroacetic compounds which comprises converting a 1,1-diflouro-1,2-dibromodihaloethane with oleum having 50-70% SO3 to a bromodifluoroacetyl halide (bromide or chloride) and then in reacting the latter directly with either an alcohol, or with water.

There is provided a process for producing 3,3,3-trifluoropropionyl chloride, which is characterized in that 3,3,3-trifluoropropionaldehyde is chlorinated by a chlorinating agent selected from the group consisting of chlorine (Cl2), sulfuryl chloride (SO2Cl2) and organic N-chloro compounds.

The invention discloses a treatment method of perfluoroalkyl acyl fluoride waste. The method comprises the following steps of: first, adding aqueous alkali to the perfluoroalkyl acyl fluoride waste, adjusting the pH value to 7-8, standing and separating to obtain a water phase and an oil phase; then, separating and purifying the water phase to obtain perfluorocarboxylate; and finally, separating and purifying the oil phase to obtain inertial fluorocarbon. The perfluoroalkyl acyl fluoride waste is treated in grades in the following steps of: adding aqueous alkali to separate the perfluoroalkyl acyl fluoride waste into the water and oil phases, and respectively separating and purifying the water and oil phases; and obtaining high purity perfluorocarboxylate after separation and purification of the water phase and obtaining high purity inertial fluorocarbon after separation and purification of the oil phase. The treatment condition is mild and the treatment effect is good.

An C-acetate preparation method comprises the following steps: adopting methyl magnesium bromide or methyl magnesium chloride as precursor, reacting the precursor with CO2 in a Loop to prepare an intermediate C-acetyl bromine or magnesium chloride adduct; without adopting purification process, injecting N2 and removing tetrahydrofuran (THF), adding water in the mixture, injecting the mixture through integral small columns (C18 small column, SEP-PAK TSCX small column and SEP-PAK TIX small column) in turn for isolation and purification where the intermediate C-acetyl bromine or magnesium chloride hydrolyzes, filtrating by aseptic filter membrane, neutralizing by alkaline solution and obtaining C-AC parenteral solution. The preparation method of the invention has the advantages of the realization of column hydrolysis and purification, fully automatic synthesis, short synthesis time, high radiochemical yield, high radiochemical purity and low production cost.

The invention provides a method for recycling trimethylacetic acid from pivaloyl chloride rectification raffinate. According to the technical scheme, the method has the experiment ideas that components and contents of pivaloyl chloride rectification raffinate are analyzed firstly on the basis of experiment means, on the basis, procedures such as hydrolysis, layering and rectification are confirmedaccording to chemical properties of pivaloyl chloride and trimethylacetic anhydride, and trimethylacetic acid is recycled. Specifically, the method comprises the following steps: firstly, adding a certain amount of pivaloyl chloride rectification raffinate, controlling specific temperature and pressure, adding a proper amount of water for hydrolysis reactions for multiple times to sequentially convert pivaloyl chloride and trimethylacetic anhydride into trimethylacetic acid, leaving to stand to layer water-containing phosphorous acid and a crude trimethylacetic acid product, feeding back thecrude trimethylacetic acid product to a trimethylacetic acid rectification procedure, and performing decoloring refining. By adopting the method provided by the invention, more than 90% of the pivaloyl chloride rectification raffinate can be converted into trimethylacetic acid, so that the utilization rates of raw materials are increased, the wastes are reduced, the environment protection burden of companies is alleviated, and meanwhile the production cost of products is effectively reduced.

A catalyst for producing from an olefin the corresponding unsaturated aldehyde and unsaturated carboxylic acid in good yield, and a process for its production, are presented.It is a composite oxide catalyst containing at least molybdenum, bismuth and iron, to be used at the time of gas phase catalytic oxidation of an olefin with a molecular oxygen-containing gas to produce the corresponding unsaturated aldehyde and unsaturated carboxylic acid, wherein the loss on drying of the contained moisture, as represented by the following formula (1) (wherein W1 represents the weight when the catalyst is heated for two hours at 110±5° C., and W2 represents the weight of the catalyst prior to such heating), is at most 0.5 wt %:Loss on drying=(W2−W1) / W2×100.  (1)

A process for recycling a polymer blend necessarily containing PLA, comprising grinding, compacting, dissolving in a solvent of PLA, removing the undissolved contamining polymers, alcoholysis depolymerisation reaction and purification steps.

A fluorocarboxylic acid preparation process which includes hydrolyzing fluorocarboxylic acid fluoride in the presence of an aqueous sulfuric acid solution to form a reaction product containing a fluorocarboxylic acid and hydrogen fluoride (present as hydrofluoric acid); and removing at least some of the hydrogen fluoride from the reaction product by washing the reaction production with aqueous sulfuric acid solution. The hydrolyzing and washing are carried out at a temperature at which the fluorocarboxylic acid is a liquid.

The invention relates to a fluorine-containing polymer for photoresist, a top anti-reflection film composition containing the fluorine-containing polymer and application of the fluorine-containing polymer in the photoresist. The structural formula of the fluorine-containing polymer for the photoresist is CF2(CF3)CF2-[O-CF(CF3)CF2]n-O-CF(CF3)COO-R, wherein n is in a range of 1-8, and R is one or more selected from the group consisting of H, NH4 or other similar structures. On the basis of the weight of the whole polymer, the content a of a polymer component with n of no more than 1 is 0-12%; the content b of a polymer component with n of 2 is 55-80%; the content c of a polymer component with n of 3 is 15-30%; the content d of a polymer component with n of 4 is 0-15%; the content e of a polymer component with n of no less than 5 is 0-8%, wherein the sum of b and c is no less than 80%; and a, d and e are equal to 0 at the same time, or any one of a, d and e is equal to 0, or a, d and e are not equal to 0 at the same time. By controlling the content distribution of the polymer components with different molecular weights in the fluorine-containing polymer, the fluorine-containing polymer meeting specific composition requirements is obtained; and the fluorine-containing polymer is easy to degrade, low in toxicity and friendly to environment and can be used for preparing a top anti-reflection film with a low refractive index.