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Method for recycling veratraldehyde production wastewater

A technology for producing waste water and veratraldehyde, applied in chemical instruments and methods, applications, inorganic chemistry, etc., can solve problems such as environmental pollution, waste, and ineffective utilization

Inactive Publication Date: 2019-09-06
江苏绿洲化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the reaction process, phosphorus-containing organic wastewater is produced, which cannot be effectively used, resulting in great waste and polluting the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A method for recycling waste water produced by veratraldehyde, comprising the steps of preparation of veratraldehyde, recovery of waste water, and utilization of waste water,

[0018] a, the preparation of veratraldehyde:

[0019] Add 600kg of veratrole, 700kg of N-methyl-formanilide, 700kg of phosphorus oxychloride into a 3000L glass-lined reactor, stir at 30-50 degrees, keep warm for 2 hours, then heat up to 80-90 degrees for 2 hours After the reaction is complete, add 1000L water for hydrolysis, stir for 30 minutes, let stand, and separate layers. The upper oil layer is the product oil. After vacuum distillation, about 650kg veratraldehyde can be obtained, and the lower layer of water layer is divided into a 2000L stirring tank. ,

[0020] b. Recycling of waste water:

[0021] Pour liquid ammonia into the stirred tank in step a, adjust the pH to 7-8, add 184kg of magnesium oxide, stir for 1 hour, centrifuge, the filter cake is magnesium ammonium phosphate, wash wit...

Embodiment 2

[0026] The preparation method of veratraldehyde:

[0027] Add 600kg of veratrole, 700kg of N-methyl-formanilide, and 700kg of phosphorus oxychloride into a 3000L glass-lined reactor, stir at 40°C, keep warm for 2 hours, then heat up to 85°C for 2 hours, and the reaction is complete. Add 1000L water for hydrolysis reaction, stir for 30 minutes, let stand, and separate layers. The upper oil layer is the product oil. After vacuum distillation, 660kg veratraldehyde can be obtained, with a yield of 91%. In a glass reactor, feed liquid ammonia to pH 7.5, add 184kg of magnesium oxide, stir for 1 hour, centrifuge, collect the water layer and use it for the previous hydrolysis reaction, the filter cake is magnesium ammonium phosphate, washed with a small amount of water, 70 degrees Vacuum drying yielded 1100kg magnesium ammonium phosphate.

[0028] After the waste water is reused 4 times, the waste water is cooled to 0 degrees, crystals are precipitated, centrifuged to obtain ammonium...

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PUM

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Abstract

The invention relates to a method for recycling veratraldehyde production wastewater. The method comprising the following steps: a, preparing veratraldehyde: adding 600 kg of verazone, 700 kg of N-methylformanilide and 700 kg of phosphorus oxychloride into a 3000 L glass-lined reactor, performing stirring, carrying out a heat insulation reaction at 30-50 DEG C for 2 h, raising the temperature to 80-90 DEG C, carrying out a reaction for 2 h, adding 1000 L of water after the reaction is completed in order to carry out hydrolysis, stirring the obtained solution for 30 min, standing for layering the solution to obtain an upper oil layer that is product oil, carrying out reduced pressure distillation on the product oil to obtain about 650 kg of the product, and separating the obtained lower water layer into a 2000 L stirring kettle; b, recovering wastewater: introducing liquid ammonia into the stirring kettle in step a to adjust the pH value of the lower water layer to 7-8, adding 184 kg ofmagnesium oxide, performing stirring for 1 h, centrifuging the obtained solution, and collecting the veratraldehyde production wastewater; and c, utilizing the wastewater: using the water recovered in step b in the hydrolysis reaction in the step a.

Description

technical field [0001] The invention relates to a method for reusing chemical waste water, in particular to a method for reusing waste water to synthesize veratraldehyde by using veratrol as a raw material. Background technique [0002] Veratraldehyde, also known as methyl vanillin, methyl vanillin, chemical name 3,4-dimethoxybenzaldehyde, CAS number: 120-14-9, molecular formula C9H10O3, molecular weight 166.17, white to brown yellow crystal , a sweet woody and perfume herb aroma, a strong vanilla-like sweetness, a melting point of 43-45 degrees, almost insoluble in cold water, soluble in hot water, ethanol and oils, is an important synthetic fragrance , is also an important pharmaceutical intermediate. [0003] In the process of synthesizing veratraldehyde by Vilsmeier reaction with veratrol as raw material, DMF or N-methyl-formanilide is usually used as formylating reagent, and phosphorus oxychloride is Lewis acid. The acylating reagent reacts with phosphorus oxychloride...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45C01C1/16C05B7/00C05C3/00C07C45/51C07C47/575
CPCC01B25/451C01C1/164C05B7/00C05C3/00C07C45/516C07C47/575
Inventor 徐兵夏铁红夏铁平夏治海
Owner 江苏绿洲化工有限公司