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US 2025/0129002 A1Published application
Production method of product 1,3-butylene glycol
AssigneeKH Neochem Co., Ltd.
InventorsKouji KURAMOTO, Yuki TACHIBANA, Hirotaka TANAKA
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Abstract
A method for producing a product 1,3-butylene glycol, including a step of subjecting crude 1,3-butylene glycol to hydrogenation treatment using a Pd/C catalyst.
Claims4
A method for producing a product 1,3-butylene glycol, comprising:
- a step of subjecting crude 1,3-butylene glycol to hydrogenation treatment using a Pd/C catalyst.
A product 1,3-butylene glycol, wherein an area percentage of a peak of 1,3-butylene glycol in a gas chromatography analysis under the following conditions is 99.5% or more, and a weight fraction of a dinitrophenylhydrazine derivative of 6-hydroxy-2-hexanone in an HPLC analysis under the following conditions is 18.0 ppm or less,
- wherein the conditions of the gas chromatography analysis are as follows:
- analysis column:
- a column in which polyethylene glycol is used as a stationary phase (length of 30 m×inner diameter of 0.25 mm×film thickness of 0.25 μm),
- temperature rising conditions:
- a temperature is raised from 80° C. up to 230° C. at 5° C./minute and then retained at 230° C. for 10 minutes,
- sample introduction temperature:
- 250° C.,
- carrier gas:
- nitrogen,
- gas flow rate in column:
- 0.5 mL/minute,
- detector and detection temperature:
- flame ionization detector (FID) and 250° C.,
- control mode:
- constant flow
- split ratio:
- 50:1,
- sample injection condition:
- 1 μL, and
- wherein the conditions of the HPLC analysis are as follows:
- the sample preparation is as follows:
- 1000 μL of a solution of 2,4-dinitrophenylhydrazine, which is extracted by adding 5 mL of acetonitrile to a cartridge packed with spherical silica gel coated with 2,4-dinitrophenylhydrazine, and 100 μL of 0.2 mol/L hydrochloric acid are added to 0.05 g of the product 1,3-butylene glycol, and a resultant mixture is reacted at 45° C. for two hours.
- (Analysis Conditions)
- Measurement sample:
- a reaction liquid obtained by the sample preparation is diluted to 2 mL with a mobile phase that is used in HPLC, and the diluted liquid is used as a measurement sample,
- Detector:
- UV-Vis detector,
- Detection wavelength:
- 369 nm,
- Analysis column:
- a column in which palmitamidopropyl group-modified silica gel (particle diameter:
- 5 μm, inner diameter×length=4.6 mm×25 cm, pore size:
- 100 Å, surface coating level:
- 2.7 μmol/m2, surface area:
- 450 m2/g, metal impurity:
- less than 5 ppm, carbon content:
- 19.5%) is used as a stationary phase,
- Column temperature:
- 40° C.,
- Mobile phase:
- acetonitrile/distilled water=50/50 (volume ratio),
- Mobile phase flow rate:
- 0.4 mL/min,
- Sample injection amount:
- 20 μL
42 more elements
Dependencies are inferred from the claim text.