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Production method of diethyl phthalate for flavors and fragrances

A technology of diethyl phthalate and a production method is applied in the production field of diethyl phthalate for flavors and fragrances, and can solve problems such as difficulty of diethyl phthalate and the like

Inactive Publication Date: 2015-09-30
RUNTAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, it is difficult to obtain odorless and high content of diethyl phthalate

Method used

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  • Production method of diethyl phthalate for flavors and fragrances
  • Production method of diethyl phthalate for flavors and fragrances
  • Production method of diethyl phthalate for flavors and fragrances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A. Basic feeding formula

[0027] Phthalic anhydride 12500kg national standard superior product, in line with GB / T15336-2006

[0028] Ethanol 5500kg density is 0.83-0.86g / cm 3 (made by fermenting corn)

[0029] Concentrated sulfuric acid 36kg national standard superior product, in line with GB / T534-2002

[0030] B. Specific operation steps

[0031] 1. Mixing materials: first add ethanol to the mixing tank, the amount of ethanol is 35% of the total ethanol weight, start stirring, if the temperature is too low, use steam to heat up slowly, but the temperature must not exceed 50°C, gradually add 12500kg of phthalic anhydride in the mixing tank. After adding the phthalic anhydride and stirring for 30 minutes, the mixture was transferred to the esterification tank.

[0032] 2. Esterification: After all the mixture is input into the esterification kettle, start stirring, then add 36kg of sulfuric acid, slowly open the steam valve, slowly raise the temperature, fully refl...

Embodiment 2

[0043] A, the basic formula for feeding

[0044] Phthalic anhydride 12500kg national standard superior product conforms to GB / T15336-2006

[0045]Ethanol 5500kg density is 0.83-0.86g / cm 3 (made by fermenting corn)

[0046] Concentrated sulfuric acid 40kg national standard superior product conforms to GB / T534-2002

[0047] B. Specific operation steps

[0048] 1. Mixing materials: first add ethanol to the mixing tank, the amount of ethanol is 45% of the total ethanol weight, start stirring, if the temperature is too low, use steam to heat up slowly, but the temperature must not exceed 50°C, gradually add 12500kg of phthalic anhydride in the mixing tank. After adding the phthalic anhydride and stirring for 30 minutes, the mixture was transferred to the esterification tank.

[0049] 2. Esterification: After all the mixture is input into the esterification kettle, start stirring, then add 36kg of sulfuric acid, slowly open the steam valve, slowly raise the temperature, fully r...

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Abstract

The invention relates to a production method of diethyl phthalate for flavors and fragrances, which comprises the following steps: mixing phthalic anhydride, ethanol and concentrated sulfuric acid, carrying out esterification reaction to the esterification end point, removing the unreacted ethanol, washing, standing separating, transferring the obtained product to a distillation kettle, heating to 120 DEG C, carrying out steam distillation under the vacuum degree of 0.096-0.1 MPa for 1-1.5 hours, heating to 160-170 DEG C, and collecting the distillate in such stage. When the obtained diethyl phthalate is used as a fixative for flavors and fragrances, the product content is 99.9% above according to the requirement, the water content is lower than or equal to 500ppm, and the acid number is lower than or equal to 0.1mg KOH / g, and thus, the diethyl phthalate does not have any smell and satisfies the requirements for preparing flavors and fragrances on the premise of satisfying the conditions above.

Description

technical field [0001] The invention relates to a method for producing diethyl phthalate for flavors and fragrances, in particular to a method for producing high-purity diethyl phthalate for flavors and fragrances. Background technique [0002] Diethyl phthalate, English name Diethyl Phthalate, referred to as DEP. Molecular formula: C 12 h 14 o 4 , Molecular weight: 222.24, it can be used as a plasticizer, solvent, lubricant, fixative, foaming agent for flotation of non-ferrous or rare metal mines, and stationary liquid for gas chromatography. [0003] In the flavor and fragrance industry, diethyl phthalate is used as a fixative, and the product content is required to be above 99.9%, moisture ≤ 0.05%, and acid value ≤ 0.1mgKOH / g. If the above conditions are met, it must not contain any odor. Because there are hundreds of fragrance types of flavors and fragrances, these fragrance types are all formulated by perfumers based on experience and sense of smell, and the fixative...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/80C07C67/08C07C67/54
Inventor 张世元於宁
Owner RUNTAI CHEM CO LTD
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