34results about How to "Simple and safe process operation" patented technology

The invention relates to a method for removing sulfur in petroleum coke and a desulfurizer thereof. The method adopts two types of mixed acid with a fixed ratio controlled as the desulfurizer, and comprises the following steps: placing fine petroleum coke with a high S content (the S content being 3-7 percent) in the mixed acid under the atmospheric pressure and the temperature of 0-60 DEG C, soaking the petroleum coke for reaction for a certain time, separating the petroleum coke and the soaking solution, washing and drying. The desulfurization percent of the obtained petroleum coke is 45-60 percent, the microstructure of the petroleum coke is not changed obviously, and the separated soaking solution of mixed acid can be repeatedly used when being mixed with the newly prepared liquid. The method has the advantages of low desulfurization cost, simple operation and significant desulfurization effect.

The invention discloses a method for synthesizing perfluoroisobutyronitrile. According to the method, industrialized products including hexafluoropropylene and chloroformic ester are used as raw materials to prepare a product; a reaction route comprises the following steps: synthesizing heptafluoroisobutyrate through the hexafluoropropylene and the chloroformic ester under the action of fluoride through a one-pot method; taking the heptafluoroisobutyrate and ammonia to react to obtain heptafluoroisobutyramide; dehydrating the heptafluoroisobutyramide through a dehydrating agent, and rectifyingand purifying to obtain the perfluoroisobutyronitrile (2,3,3,3-tetrafluoro-2-trifluoromethylpropionitrile). According to the method disclosed by the invention, the used raw materials are commerciallyavailable; the main raw materials including the chloroformic ester and the hexafluoropropylene have low cost and can be abundantly supplied; reaction conditions are moderate and the reaction conversion rate and the yield are high; the product of each step is easy to separate and the purity of the product is high; the method has the advantages of convenience and safety in operation of a technologyand easiness for realizing industrial production.

The invention discloses an environment-friendly water-based automobile shellac cleaning agent. The environment-friendly water-based automobile shellac cleaning agent consists of the following components: fatty alcohol-polyoxyethylene ether phosphate, limonene, fatty acid diethanol amide, sodium carbonate and deionized water. The cleaning agent is prepared by compounding various non-toxic surfactants with excellent biodegradability and aids, has obvious synergistic effect among the components, can effectively remove shellac dirt form the surface of the automobile and has a good anti-rust effect on metal. The production method is simple to operate and low in production cost, and has good environmental and economic value.

The invention provides a method for preparing phospholipids type DHA through catalysis of a biological enzyme. The method includes the step of preparing phospholipids type DHA from phospholipids and substances with DHA through catalysis of the biological enzyme. DHA grease does not need to be dissociated into dissociative docosahexaenoic acid (DHA) in advance, the process operation is simple and safe, reaction byproducts are few, lots of products can be rapidly obtained after one-time operation, the operation process is simplified, and the investment of devices is reduced.

The present invention provides an extracting and purifying method for improving the yield of SDG, and creates a SDG sequential extracting and purifying scheme based on the method. The technical route of the present invention is that operations of microbial fermentation, enzymatic degradation, and non-salt process are integrated in the SDG extracting and purifying technology process based on the prior art, thus greatly improving the efficiency of SDG extracting and purifying and lowering the manufacturing cost. The present invention also creates a SDG graded purifying process to prepare products, whose purities are respectively 8 to 10 percent, 20 to 40 percent, 50 to 60 percent, as well as 90 percent. The front two products need not column chromatographic separation, and the process operation is simple and safe, thus the present invention is economical and practical, and is suitable to the industrial production; the present invention can satisfy the needs of functional food ingredient and health food; later two products have mature technology, stable technology process, and high product purity, thus being able to satisfy the needs of pharmacological study and drug development.

The invention provides a medical titanium implant micro-arc oxidation film layer and a preparation method. The medical titanium implant micro-arc oxidation film layer comprises a matrix and an oxidization film layer formed on the surface of the matrix, wherein a plurality of micro holes are distributed in the surface of the oxidization film layer; the micro holes consist of a plurality of micro bosses and grooves; the bosses are inwards sunken to form concave holes; the grooves are distributed in the peripheries of the bosses; the bosses are protruded relative to the grooves; the grooves are in an irregular state; the adjacent grooves are communicated with each other; and the oxidation film layer has color. The film layer provided by the invention has hydrophilicity, high-strength binding force and color. The medical titanium implant micro-arc oxidation film layer is simple in operation and preparation process, is relatively low in cost, and the obtained film layer is excellent in performance, and is suitable for industrial production.

The invention discloses a preparation method of tetraethyl methylene diphosphate, comprising the following steps: 1) under the action of sodium ethoxide, diethyl phosphite reacts with sodium ethoxide to obtain sodium diethyl phosphite ethanol solution , ethanol is removed by distillation under reduced pressure to obtain sodium diethyl phosphite solid; 2) dichloromethane is added to the solid sodium diethyl phosphite obtained in step 1); sodium diethyl phosphite and dichloromethane are substituted After the reaction, tetraethyl methylene diphosphate was obtained. The preparation method of the invention has mild and simple reaction conditions and high yield at the same time. The method is simple to operate and low in energy consumption, and is suitable for industrial production.

The invention relates to a method for producing a flame-retardant fiber from a vinylon production line and an obtained flame-retardant fiber. The method comprises the following steps: a) dissolving polyvinyl alcohol in water so as to obtain a spinning solution; b) adding an aqueous solution of a tetrahydroxymethyl phosphorus compound; c) spinning by using a mirabilite wet method, and performing condensation and stretching so as to obtain a primary fiber; d) drying the primary fiber obtained in the step c) so as to obtain a flame-retardant precursor fiber; e) performing ammonia fumigation on the flame-retardant precursor fiber obtained in the step d) so as to obtain an ammonia fumigation fiber; f) oxidizing the ammonia fumigation fiber obtained in the step e); and g) randomly performing washing, oiling and drying, thereby obtaining the flame-retardant fiber.

The invention discloses a synthetic method of anti-tumor molecular targeted drug crizotinib, belongs to the field of pharmaceuticals, and relates to a synthetic method of a crizotinib intermediate. The method comprises two reduction processes: a bromination reaction process comprises the following reaction steps: a reduction process I: carrying out reduction reaction on a (R)-3-[1-(2,6-dichloro-3-fluorophenyl)ethoxyl]-2-nitropyridine compound and sodium dithionate under a mechanical chemical condition to generate (R)-3-[1-(2,6-dichloro-3-fluorophenyl)ethoxyl]-2-aminopyridine; a reduction process II: dissolving the (R)-3-[1-(2,6-dichloro-3-fluorophenyl)ethoxyl]-2-nitropyridine compound into an organic solvent, carrying out catalytic hydrogenation and reduction treatment to generate (R)-3-[1-(2,6-dichloro-3-fluorophenyl)ethoxyl]-2-aminopyridine; the bromination reaction process comprises a step of carrying out reaction between the compound and potassium hydrogen persulfate as well as bromate to obtain the crizotinib intermediate. The process is low in cost, the raw materials are easy to purchase, the operation is simple, convenient and safe, and the yield is high; moreover, the process is suitable for large-scale production.

The invention discloses a method for preparing long-chain fluoroalkylsiloxane. According to the method, long-chain fluoroalkylethylene and alkoxy silane are used as raw materials to prepare the long-chain fluoroalkylsiloxane through hydrosilylation. The method is characterized in that a hexafluoroisopropanol solution of chloroplatinic acid is used as a catalyst and the dosage of a platinum catalyst is 10<-5> to 10 <-4> of the molar amount of the alkoxy silane. The method comprises the following steps: under the protection of nitrogen, adding hexafluoroisopropanol into chloroplatinic acid hexahydrate to completely dissolve chloroplatinic acid so as to prepare a chloroplatinic acid / hexafluoroisopropanol solution with a concentration of 1-10 mM; sequentially adding alkoxy silane, long-chain fluoroalkylethylene and the prepared chloroplatinic acid / hexafluoroisopropanol solution into a reactor, and conducting reacting at 40-80 DEG C for 30-60 minutes; and carrying out reduced-pressure distillation on reaction liquid to obtain the target product, namely long-chain fluoroalkylsiloxane. The method is simple in process, mild in reaction conditions and high in product yield and purity.

The invention relates to a method for preparing a key intermediate 4-methyl-5-ethoxazole of vitamin B6 and belongs to the technical field of crude drug preparation. The method for preparing 4-methyl-5-ethoxazole comprises the steps that firstly, 4-methyl-5-ethyoxyl-1,3-oxazole-2-nonanoic acid-ethyl ester, methylbenzene, drinking water and sodium hydroxide are sequentially put into a hydrolysis reaction still according to a certain proportion, and stirring, heat preservation and reacting are carried out; liquid separation is carried out, and the pH value of the water phase is adjusted to rangefrom 1.0 to 2.5; an organic solvent is added to the system obtained in the second step, reacting is carried out by controlling the temperature ranging from 30 DEG C to 50 DEG C until no carbon dioxideis generated; after decarboxylation is finished, the pH value is adjusted to be larger than or equal to 9.0, liquid separation is carried out, the organic phase is subjected to vacuum distillation, and 4-methyl-5-ethoxazole is obtained. The process is easy and safe to operate, and industrial production is easy.

The invention provides a preparation method of 2-chloro-5-nitropyridine. The preparation method comprises the following steps: preparing 2-hydroxy-5-nitropyridine by taking 2-nitroacetaldehyde diethylacetal as an initial raw material through two methods; and then carrying out a chlorination reaction on the 2-hydroxy-5-nitropyridine and a chlorination reagent to prepare the 2-chloro-5-nitropyridine. The method has the advantages of cheap and accessible raw materials and low cost, does not use a diazotization hydrolysis reaction, is safe, simple and convenient to operate, does not use mixed acid, is less in wastewater yield and environmentally-friendly, does not use a nitration reaction, is high in reaction selectivity, few in side reactions, simple in post-treatment and high in product yield and product, and is suitable for industrial production.

The invention discloses a synthesis method of heptafluoroisobutyronitrile, which comprises the following steps: (1) reacting hexafluoropropylene with carbon dioxide under the catalysis of fluoride salt to obtain heptafluoroisobutyrate; (2) acidifying the obtained heptafluoroisobutyric acid, and then carrying out esterification reaction with alcohol to obtain heptafluoroisobutyrate; and (3) reacting the obtained heptafluoroisobutyrate with ammonia, and dehydrating to obtain heptafluoroisobutyronitrile. The synthesis method has the advantages of easily available raw materials, mild reaction conditions, high reaction conversion rate and yield, easy separation and purification, simple and safe process operation, short synthesis route and low cost.

The invention provides a medical titanium implant micro-arc oxidation film layer and a preparation method. The medical titanium implant micro-arc oxidation film layer comprises a matrix and an oxidization film layer formed on the surface of the matrix, wherein a plurality of micro holes are distributed in the surface of the oxidization film layer; the micro holes consist of a plurality of micro bosses and grooves; the bosses are inwards sunken to form concave holes; the grooves are distributed in the peripheries of the bosses; the bosses are protruded relative to the grooves; the grooves are in an irregular state; the adjacent grooves are communicated with each other; and the oxidation film layer has color. The film layer provided by the invention has hydrophilicity, high-strength binding force and color. The medical titanium implant micro-arc oxidation film layer is simple in operation and preparation process, is relatively low in cost, and the obtained film layer is excellent in performance, and is suitable for industrial production.

The invention provides a method for continuously extracting durene from coal-sourced aromatic hydrocarbon. The method comprises the steps: adding a coal-sourced aromatic hydrocarbon raw material intoa primary distillation tower, separating light components such as trimethylbenzene in the raw material from the top of the primary distillation tower by utilizing the negative pressure inside the primary distillation tower, and placing the light components into a light component storage tank by a heat radiator; making a residual tower bottom in the primary distillation tower enter a rectifying tower to obtain a durene-enriched solution with the mass percentage of 90%-95% at the top of the rectifying tower; and storing the durene-enriched solution into a middle durene storage tank, and then, delivering the durene-enriched solution into a multistage crystallizer for fractional crystallization to refine durene with the purity of 99% or above. By using the method, the purity of durene can be increased to 99% or above, a product is a white powdery / sheet-like crystal, and the conversion ratio of the product can be increased by 5%-10% during downstream pyromellitic dianhydride processing. Compared with a traditional freezing-centrifuging-squeezing process, the method is simple and safe in process operation and low in energy consumption and risk; and the method can be used for processing durene with different contents according to market demands, so that the market demands are met.

The invention provides a method for preparing phospholipids type DHA through catalysis of a biological enzyme. The method includes the step of preparing phospholipids type DHA from phospholipids and substances with DHA through catalysis of the biological enzyme. DHA grease does not need to be dissociated into dissociative docosahexaenoic acid (DHA) in advance, the process operation is simple and safe, reaction byproducts are few, lots of products can be rapidly obtained after one-time operation, the operation process is simplified, and the investment of devices is reduced.

The invention discloses a preparation method of 3,4-diacetoxy-1-butene. The preparation method comprises steps as follows: an esterification step: 1,4-butylene glycol and acetic acid are subjected to an esterification reaction in the presence of acid, a solution containing 1,4-diacetoxy-2-butene and acetic acid is obtained, acetic acid is removed and 1,4-diacetoxy-2-butene is obtained; an isomerization step: cuprous catalysts are added to 1,4-diacetoxy-2-butene obtained in the esterification step, the mixture is heated for an isomerization rearrangement reaction, and a mixed solution containing 3,4-diacetoxy-1-butene is obtained; a purification step: the mixed solution obtained in the isomerization step is purified, and 3,4-diacetoxy-1-butene is obtained. The preparation method adopts easy-to-realize reaction conditions and has the characteristic of high yield.

The invention relates to a preparation method of anidulungin side chain intermediate p-amyloxy terbenzoic acid. The method comprises the following steps: S1: 4-hydroxy-4'-bromobiphenyl and 1-bromopentane undergo a nucleophilic substitution reaction to obtain 4'-bromo-4-n-pentyloxybiphenyl; S2: 4'-bromo ‑4‑pentyloxybiphenyl and tetrahydroxydiboron undergo Suzuki coupling reaction to obtain 4‑pentyloxy‑4'‑biphenylboronic acid; S3: 4‑pentyloxy‑4'‑biphenylboronic acid and 4‑ Methyl iodobenzoate undergoes a Suzuki coupling reaction to obtain methyl 4''-(pentyloxy)-[1,1',4',1''-terphenyl]-4-formate; S4: hydrolysis to obtain p- Pentoxy terbenzoic acid. The present invention adopts Suzuki coupling to prepare aryl boronic acid and then prepares the target product through Suzuki coupling and alkali hydrolysis, which has the advantages of low cost, simple and safe process operation.

The invention relates to a method for removing sulfur in petroleum coke and a desulfurizer thereof. The method adopts two types of mixed acid with a fixed ratio controlled as the desulfurizer, and comprises the following steps: placing fine petroleum coke with a high S content (the S content being 3-7 percent) in the mixed acid under the atmospheric pressure and the temperature of 0-60 DEG C, soaking the petroleum coke for reaction for a certain time, separating the petroleum coke and the soaking solution, washing and drying. The desulfurization percent of the obtained petroleum coke is 45-60percent, the microstructure of the petroleum coke is not changed obviously, and the separated soaking solution of mixed acid can be repeatedly used when being mixed with the newly prepared liquid. The method has the advantages of low desulfurization cost, simple operation and significant desulfurization effect.

The invention discloses potentilla discolor bunge teabags with the effect of reducing blood sugar and lipids and a preparation method for the potentilla discolor bunge teabags, and belongs to the technical field of blood processing. The preparation method comprises the following steps: separating roots, stems and leaves of potentilla discolor bunge, performing extraction with different solvents respectively, mixing extracting solutions, performing reduced-pressure concentration to obtain a whole-herb extracting solution of the potentilla discolor bunge, and collecting extracted root particles as carriers; uniformly stirring and mixing the whole-herb extracting solution and the carriers, and performing baking and frying until flavor is disseminated; and cooling and quantitatively bagging the mixture to obtain potentilla discolor bunge teabag finished products. According to the method, the stems, leaves and roots of the potentilla discolor bunge are extracted with different solvent systems respectively, so that the extraction rate of active substances is increased; the extracted root particles are adopted for adsorbing extracts as the carriers, so that the functional activity of the plants is greatly developed; the prepared teabags have remarkable DPP-4 suppression activity, and have the effects of reducing blood sugar and lipid levels, promoting insulin secretion and alleviating diabetes; a process is easy to operate, and the finished products are brown in color, rich in aroma and suitable for industrial production.

The invention relates to a method for producing a flame-retardant fiber from a vinylon production line and an obtained flame-retardant fiber. The method comprises the following steps: a) dissolving polyvinyl alcohol in water so as to obtain a spinning solution; b) adding an aqueous solution of a tetrahydroxymethyl phosphorus compound; c) spinning by using a mirabilite wet method, and performing condensation and stretching so as to obtain a primary fiber; d) drying the primary fiber obtained in the step c) so as to obtain a flame-retardant precursor fiber; e) performing ammonia fumigation on the flame-retardant precursor fiber obtained in the step d) so as to obtain an ammonia fumigation fiber; f) oxidizing the ammonia fumigation fiber obtained in the step e); and g) randomly performing washing, oiling and drying, thereby obtaining the flame-retardant fiber.

The invention relates to a preparation method of soft biomass automobile washing liquid and belongs to the technical field of automobile cleaning and care articles. Milk fat is hydrolyzed under the acidic environment to produce higher fatty acid, the higher fatty acid is reduced into higher fatty acid alcohol under the action of reducing oxalic acid, the higher fatty acid alcohol reacts with glucose at high temperature to generate glycerinum and decyl glucoside, elements such as nitrogen, sulfur and phosphorus in chicken liver extracting liquid and the glycerinum are subjected to synergistic action to form one layer of chemical protective film on the surface of an automobile body to protect the automobile body and have a glazing effect, lecithin in yolk and the decyl glucoside serving as surfactants have strong detersive powder and rich foam and are fine and stable, and tea saponin and tea polyphenol in the tea extracting liquid have oxidation resistance and can improve the storage stability of the automobile washing liquid. The automobile washing liquid prepared by the method has obvious synergistic effect, is non-toxic, low in irritation and rapid and complete in biodegradation, avoids corrosion to the automobile body, and has excellent application prospect.

The invention relates to a preparation method of 4-methyl-5-ethoxyxazole, a key intermediate of vitamin B6, and belongs to the technical field of preparation of raw materials. The preparation method of 4-methyl-5-ethoxyxazole described in the present invention, first in the hydrolysis reaction kettle, drop into 4-methyl-5-ethoxyl-1,3-oxazole-2 sequentially in a certain proportion ‑Ethyl carboxylate, toluene, drinking water and sodium hydroxide, stir and keep warm for reaction; separate liquid, use hydrochloric acid to adjust the pH value of the aqueous phase in the range of 1.0‑2.5; add organic solvent to the system obtained in the second step, 30‑50 °C Control the temperature and react until no carbon dioxide is released; after decarboxylation, adjust the pH value to ≥9.0, separate the liquids, and distill the organic phase under reduced pressure to obtain the intermediate 4-methyl-5-ethoxyoxazole. The technological operation is simple and safe, and the industrial production is easy.

The invention discloses a preparation method of 3-(difluoromethyl)-1-methyl-1H-pyrazol-4-carboxylic acid. The reaction formula is shown in the specification. Difluoroacetic acid, which is relatively low in price and small in molar mass and is introduced at a post-synthesis phase is adopted, so that the preparation method of the 3-(difluoromethyl)-1-methyl-1H-pyrazol-4-carboxylic acid is low in cost, simple and safe in technological operation, high in product content, and high in product yield; the content is 98.1-98.9% (liquid chromatogram, external standard); the total yield is 52.2-56.9% (based on propargyl alcohol). Nanoscale titanium dioxide is adopted to carry out catalytic esterification, so that the reaction yield is high; the reaction time is short; the used raw materials and solvent are cheap and available; furthermore, an organic solvent is avoided in the four reaction steps, so that the solvent recovery cost and the environmental pollution risk are greatly reduced.

The invention relates to a synthesis method of antioxidant 1076 using solid base catalyst. The 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate and the octadecanol are used as raw materials which are subjected to the interesterification reaction in the presence of a solid base catalyst to obtain the product of antioxidant 1076 with the purity more than or equal to 97.5% and the yield more than or equal to 85%. Compared with the prior art, the method provided by the invention utilizes the prepared solid base catalyst, thus the catalysis effect is improved, and the quality of obtained products is stable; in addition, the solid base catalyst is recyclable and environmental friendly, and the process operation is safe and convenient, therefore the method is suitable for the industrialized and mass production.

The invention discloses a method for synthesizing perfluoroisobutyronitrile, which is prepared by using industrial products hexafluoropropylene and chloroformate as raw materials. The reaction route is: chloroformate and hexafluoropropylene under the action of fluoride salt One-pot reaction synthesis of heptafluoroisobutyrate; heptafluoroisobutyrate reacts with ammonia to obtain heptafluoroisobutyramide; heptafluoroisobutyramide is dehydrated with a dehydrating agent and purified by rectification to obtain perfluoroisobutyronitrile ( 2,3,3,3-tetrafluoro-2-trifluoromethylpropionitrile). The raw materials selected in the method are all commercially available, and the main raw materials chloroformate and hexafluoropropylene are low in cost and can be supplied in large quantities; the reaction conditions are mild, and the reaction conversion rate and yield are high; the products of each step are easy to separate, and the product purity is high. High, simple and safe process operation, easy to industrial production.

The invention provides a preparation method of 2-chloro-5-nitropyridine. 2-Hydroxy-5-nitropyridine is prepared by two methods with 2-nitroacetaldehyde acetal as the initial raw material; then 2-hydroxy-5-nitropyridine and chlorination reagent are prepared by chlorination reaction to prepare 2-chloro ‑5‑nitropyridine. The method of the invention has cheap and easy-to-obtain raw materials and low cost; does not involve diazotization hydrolysis reaction, and is safe and convenient to operate; does not use mixed acid, produces less waste water, and is environmentally friendly; at the same time does not involve nitrification reaction, has high reaction selectivity and few side reactions , the post-treatment is simple, the product yield and purity are high, and it is suitable for industrial production.

The invention relates to the preparation method of anidulafungin side chain intermediate 4''-(pentyloxy)-[1,1':4',1''-terphenyl]-4-carboxylic acid. The preparation method includes the steps of S1, subjecting 4 hydroxy-4'-bromobiphenyl and 1-bromopentane to nucleophilic substitution to obtain 4'-bromo-4-n-amyloxybiphenyl; S2, subjecting the 4'-bromo-4-n-amyloxybiphenyl and tetrahydroxydiboron to Suzuki coupling reaction to obtain 4-pentyloxy-4'-biphenylboronic acid; S3, subjecting the 4-pentyloxy-4'-biphenylboronic acid and methyl 4-iodobenzoate to Suzuki coupling reaction to obtain methyl 4''-(pentyloxy)-[1,1',4'-1''-terphenyl]-4-formate; S4, hydrolyzing to obtain 4''-(pentyloxy)-[1,1':4',1''-terphenyl]-4-carboxylic acid. arylboronic acid is prepared through Suzuki coupling; the target product is then prepared through Suzuki coupling and alkali hydrolysis; the preparation method has the advantages of low cost and good process operation simplicity and safety.