30 results about "Dehydrolinalool" patented technology

The invention discloses a preparing method of citral. The existing method has high production cost or low yield, thus being difficult to be suitable for scale production. The method adopts dehydrogenated linalool as a raw material which is carried out with catalytic reforming to obtain the citral under the existence of a solvent and a latent solvent and is characterized in that: a catalyst adopted for reaction is molybdenum dioxide diacetyl acetone acid ester, the catalytic reforming is carried out under the existence of acid cocatalyst which is cationic exchange resin with subacidity. The catalyst and the acid cocatalyst improve the reaction yield; in addition, the catalyst and the cocatalyst can be recycled for treatment and conveniently applied mechanically, and the castlyst is environmental friendly.

The invention relates to a method to produce methyl heptenone from the production waste liquid produced by dehydrogenated linalool, and the waste liquid contains dehydrogenated linalool dimmer which is produced during the synthesizing process of the dehydrogenated linalool through ethynylation reaction of the methyl heptenone. The method comprises the processes that: the waste liquid is depolymerized in alkaline solution, the depolymerization reacting resultants is carried out oil-water phase separation, and the alkaline solution is recovered and recycled; the oil-water phase materials is distilled by steam, the oil phase materials in the gas phase condensate are collected, and the methyl heptenone is obtained. The obtained rough methyl heptenone is decompression rectified and purified, the tower top distillates between 72 to 74 DEG C are collected, and therefore the refined product is obtained. 75 to 80kg of the refined methyl heptenone products can be prepared from 100kg waste liquid. The beneficial effects of the invention is that: a green utilization method with high economic value is supplied for the waste liquid, so this part of petroleum resource can be fully used, and the exhaust of contaminants arising from the production process of the dehydrogenated linalool through the ethynylation reaction of the methyl heptenone is reduced.

It is intended to provide a fragrance composition having a natural fragrance of Jasminum sambac. This composition is a Jasminum sambac-like fragrance composition characterized by adding at least one or more components selected from the group consisting of 3,7-dimethyl-1,5-octadiene-3,7-diol, 2,6-dimethyl-1,7-octadiene-3,6-diol, and dehydrolinalool to a base composition based on a Jasminum sambac flower fragrance-like fragrance. It is preferred that the total blending amount of the fragrance components is from 0.01 to 20% by mass of the total amount of the fragrance composition.

The invention discloses a preparation and refining method for citral. The method includes: 1) in an atmospheric oxygen-free environment, taking alcohol ether as a solvent and alkylsulfone as a cosolvent, adjusting the pH value by benzoic acid or phenylacetic acid, subjecting dehydrolinalool to catalytic rearrangement under catalysis of a molybdenum acetylacetonate catalyst so as to generate citral, with the dehydrolinalool, the solvent and the cosolvent being in a mass ratio of 1:(1-4):(0.2-0.8), and with the dosage of the catalyst accounting for 2-8% of that of dehydrolinalool, controlling the pH value at 3-5, the reaction time at 3-9h, and reaction temperature at 100-125DEG C; 2) subjecting a citral-containing reaction liquid to vacuum rectification to remove light components (including the cosolvent and unreacted dehydrolinalool), with a concentrated citral solution (mainly containing citral and the solvent) left at the tower bottom, and controlling the operation pressure at 0.02-0.08MPa, the tower bottom temperature at 40-80DEG C, and the reflux ratio at 4-10; and 3) carrying out vacuum rectification on the concentrated citral solution obtained at the tower bottom to obtain a high purity citral product, which has a citral purity up to 95.7%, and controlling the operation pressure at 0.008-0.06MPa, the tower bottom temperature at 40-80DEG C and the reflux ratio at 4-10. The method provided by the invention has very obvious positive effects, makes use of the good solubility of the molybdenum catalyst in the alcohol ether solvent, not only improves the citral yield, but also realizes recycling of the catalyst dissolved in the solvent. Complex processing steps in the prior art are avoided, and the process is simplified.

The invention relates to a synthetic method of pseudoionone, which comprises the steps of sequentially performing Saucy-Marbet reaction and isomerization reaction in a microchannel reactor with dehydrolinalool and 2-methoxypropylene to prepare pseudoionone. Pseudo-ionone was prepared from dehydrolinalool through Saucy-Marbet reaction and isomerization reaction in a microchannel reactor, which realized the continuous production of pseudo-ionone with high efficiency, few reaction steps and high yield. High, high selectivity, less pollution, in line with the development concept of green chemical industry.

The invention discloses a synthesis method of ionone-type spice intermediate products, namely pseudoionone and methyl pseudoionone, wherein the pseudoionone and the methyl pseudoionone are prepared by taking dehydrogenated linalool as a raw material, reacting with a compound represented as the formula I under an appropriate catalyst condition, and implementing an isomerization reaction. The method disclosed by the invention, in preparing the ionone-type spice intermediate products, is few in reaction steps, high in yield and low in pollution, wherein the R1 represents either -H or -CH3; and R2 represents methyl, ethyl, n-propyl, isopropyl, butyl, isobutyl, 2-methyl propyl, n-amyl, isoamyl, 2-methyl butyl, benzyl or other groups.

This invention relates to a method for producing methylheptenone from dehydrolinalool production waste solution, which uses didehydrolinalool produced during the methylheptenone ethynylation reaction to synthesize dehydrolinalool, comprising: 1) the waste solution performs depolymerizing reaction in NaOH or KOH solution; 2) the reaction products perform oil-water separation and NaOH or KOH solution is recovered to be used again; 3) distill the oil-phase material with steam, and collect the gas-phase cooling liquid oil-phase material so as to obtain the crude methylheptenone; 4) purify the crude methylheptenone by depression distillation and collect the top fraction at 75-78Deg C so as to produce the refined product. This invention is characterized in that it provides a green and economic method to utilize the waste solution and make full use of this petroleum resource.

The invention discloses a preparing method of citral. The existing method has high production cost or low yield, thus being difficult to be suitable for scale production. The method adopts dehydrogenated linalool as a raw material which is carried out with catalytic reforming to obtain the citral under the existence of a solvent and a latent solvent and is characterized in that: a catalyst adopted for reaction is molybdenum dioxide diacetyl acetone acid ester, the catalytic reforming is carried out under the existence of acid cocatalyst which is cationic exchange resin with subacidity. The catalyst and the acid cocatalyst improve the reaction yield; in addition, the catalyst and the cocatalyst can be recycled for treatment and conveniently applied mechanically, and the castlyst is environmental friendly.

The invention discloses a method for rearranging and synthesizing citral by using dehydrolinalool as raw material, comprising: using dehydrolinalool as raw material, in the presence of solvent toluene and organic acid 4-tert-butylbenzoic acid, Add catalytic system MoO 2 (acac) 2 and Ph 3 PO, catalyzes the Meyer‑Schuster rearrangement to give citral. The catalyst system used in the invention can obtain citral with relatively ideal conversion rate and yield with higher activity and selectivity, and the reaction process is green and environment-friendly, without producing harmful and smelly mercaptans and thioethers. This catalytic system provides an improved method for the preparation of citral, avoids the use of sulfoxide compounds, and has a good application prospect.

The invention relates to a preparation method for citral. The method comprises the steps of: 1) in an atmospheric pressure and oxygen-free environment, and in the presence of an alcohol ether solvent and a cosolvent, using benzoic acid or phenylacetic acid to adjust the pH value in the range of 3-5, subjecting dehydrolinalool to catalytic rearrangement under the action of a Mo catalyst, keeping the dehydrolinalool, the alcohol ether solvent, and the cosolvent in a ratio of 1:2.5:0.5, with the dosage of the catalyst accounting for 5% of the weight of the dehydrolinalool, and controlling the reaction time at 5-7h and the reaction temperature at 115-120DEG C; and 2) subjecting the citral crude product obtained in step 1) to five-stage molecular distillation for separation. By making use of the good solubility of the molybdenum catalyst in the alcohol ether solvent, the method provided by the invention not only improves the citral yield, and the catalyst can be recycled due to its dissolution in the solvent. The method avoids complex processing steps in the prior art, and simplifies the process.

The invention provides a method for hydrogenation utilization of linalool rectification kettle residual liquid. According to the method, the linalool rectification kettle residual liquid with heavy components removed is taken as a raw material and is subjected to a hydrogenation reaction to synthesize dihydrolinalool or tetrahydrolinalool. According to the method, a ruthenium-carbon catalyst is used for carrying out hydrogenation reaction on the linalool rectification kettle residual liquid, and when no metal salt is added for modifying the catalyst, tetrahydrolinalool can be prepared with high selectivity; when a metal salt is added to modify the catalyst, dihydrolinalool can be prepared with high selectivity, so that productivity regulation and control of different hydrogenation productsare realized according to market demand conditions, and the method has wide actual production and application values. Besides, diamine substance can stabilize hydrogen ions at the carbon-carbon triple bond end position in the dehydrolinalool and inhibit the polymerization reaction, thereby inhibiting the generation of heavy component byproducts and being beneficial to enhancing the selectivity ofthe raw material and the yield of the product.

The invention belongs to the technical field of organic synthesis, and particularly relates to a catalyst for preparing citral through dehydrolinalool rearrangement reaction, a preparation method of the catalyst and a method for preparing the citral. The catalyst is a solid acid catalyst and comprises an active component, a carrier and an optional assistant; wherein the active component is selected from one or more of silicotungstic acid, phosphomolybdic acid and phosphotungstic acid, and the assistant is selected from one or more of gold trichloride, rhenium trichloride, indium trichloride and lanthanum trichloride. The method for preparing the citral comprises the following step of: in the presence of a solvent and the solid acid catalyst, carrying out Meyer-Schuster rearrangement reaction by taking dehydrolinalool as a raw material to prepare the citral. The solid acid catalyst is simple to prepare, low in cost and long in service life; when the catalyst is used in the process of preparing citral, the reaction yield and the conversion rate are improved, and the selectivity is good; in addition, the catalyst is long in service life, and continuous large-scale operation can be realized.

The invention provides a combined catalyst for a hotrienol rearrangement reaction for citral preparation. The catalyst is a combination of titanium tetraisopropanolate and cuprous chloride. The invention further provides a method for preparing citral through the hotrienol rearrangement reaction which adopts the catalyst combining titanium tetraisopropanolate and cuprous chloride. The catalyst is relatively high in both activity and selectivity, low in price, easy to obtain, low in dosage and very mild in reaction condition; within a relatively short reaction time, the ideal conversion rate and yield of a target product can be obtained.

The invention discloses a preparation method of citral, which uses dehydrolinalool as a raw material and molybdenum trioxide as a catalyst. In the presence of acid, citral is obtained by catalytic rearrangement in an organic inert solvent; the catalyst used in the preparation method is cheap; the amount of catalyst used is small; the catalytic efficiency is high; the reaction selectivity is good and the yield is high; Short; the catalyst can be recycled and applied.

The invention relates to a method to produce methyl heptenone from the production waste liquid produced by dehydrogenated linalool, and the waste liquid contains dehydrogenated linalool dimmer which is produced during the synthesizing process of the dehydrogenated linalool through ethynylation reaction of the methyl heptenone. The method comprises the processes that: the waste liquid is depolymerized in alkaline solution, the depolymerization reacting resultants is carried out oil-water phase separation, and the alkaline solution is recovered and recycled; the oil-water phase materials is distilled by steam, the oil phase materials in the gas phase condensate are collected, and the methyl heptenone is obtained. The obtained rough methyl heptenone is decompression rectified and purified, the tower top distillates between 72 to 74 DEG C are collected, and therefore the refined product is obtained. 75 to 80kg of the refined methyl heptenone products can be prepared from 100kg waste liquid. The beneficial effects of the invention is that: a green utilization method with high economic value is supplied for the waste liquid, so this part of petroleum resource can be fully used, and the exhaust of contaminants arising from the production process of the dehydrogenated linalool through the ethynylation reaction of the methyl heptenone is reduced.

The invention discloses a preparation method of an alpha-damascenone perfume. A technical scheme adopted by the invention is characterized in that the method comprises the following steps: 1, reacting an initial raw material dehydrolinalool with 3-bromopropylene in a mixed solvent comprising toluene and methanol to obtain 6,10-dimethylundecyl-1,9-diene-4-alkynyl-6-ol; 2, converting 6,10-dimethylundecyl-1,9-diene-4-alkynyl-6-ol obtained in step1 in a solvent comprising toluene and dimethyl sulfoxide at 90-100DEG C under the action of a catalyst to obtain fake damascenone; and 3, converting damascenone in a solvent toluene at 50-60DEG C under the action of a catalyst phosphoric acid supported on active carbon to obtain the alpha-damascenone perfume. The method has the advantages of cheap and easily available raw material, mild reaction conditions, high reaction yield of each step, recycle of the solvents comprising toluene and methanol, and low cost, and is a method suitable for the industrialized production of the alpha-damascenone perfume.