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Solid acid, preparation method thereof, solid acid-loaded micro-channel reactor, preparation method of reactor, and method for preparing hydroxycitronellal

A technology of microchannel reactor and solid acid, which is applied in the field of citronellol hydration reaction to prepare hydroxycitronellol, which can solve the problems of equipment corrosion, three wastes, low reaction conversion rate and yield, etc.

Active Publication Date: 2021-03-19
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above two process routes for preparing hydroxycitronellol have their own defects: when catalyzed with sulfuric acid, a large amount of sulfuric acid needs to be used, the recovery is difficult, and it is easy to cause corrosion of equipment, and post-treatment will produce a large amount of three wastes, causing serious environmental pollution
[0009] So far, there are many reports on the preparation of hydroxycitronellol by the hydration reaction of citronellol, but there are following defects: a large number of strong acids and organic solvents are used; the catalyst is not easy to recycle; the reaction conversion rate and yield are low; Affect product aroma quality, etc.

Method used

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  • Solid acid, preparation method thereof, solid acid-loaded micro-channel reactor, preparation method of reactor, and method for preparing hydroxycitronellal
  • Solid acid, preparation method thereof, solid acid-loaded micro-channel reactor, preparation method of reactor, and method for preparing hydroxycitronellal
  • Solid acid, preparation method thereof, solid acid-loaded micro-channel reactor, preparation method of reactor, and method for preparing hydroxycitronellal

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Preparation of solid acid a:

[0067] Chloromethylated polystyrene resin (CAS: 55844-94-5), 8-aminooctanol, 2-chloroethyl phosphoric acid, toluene, 30wt% sodium hydroxide solution according to 1:1.5:3.5:10:25 After mixing the mass proportions, reflux and stir for 1 hour, lower the temperature to 50°C, adjust the pH to about 6 with 2N hydrochloric acid solution, cool to room temperature, filter with suction, wash with deionized water until there are no chloride ions, and dry at 50°C to obtain solid acid a.

[0068] 1H NMR (300MHz, Chloroform-d) δ7.63(s,4H),7.35–7.11(m,81H),3.58–3.51(m,2H),3.51–3.43(m,2H),3.03(d,J =1.1Hz,1H),2.91–2.82(m,4H),2.81(t,J=1.0Hz,11H),2.78–2.67(m,5H),2.54(d,J=2.7Hz,2H),2.09 –1.83(m,33H),1.77(d,J=12.4Hz,1H),1.59–1.48(m,4H),1.32(dd,J=11.6,7.2Hz,8H)

[0069] The preparation of the microchannel reactor of loading solid acid a:

[0070] Solid acid a (10g), ethanol (300ml) and 0.005mol / L hydrochloric acid aqueous solution (150ml) were ultrasonicall...

Embodiment 2-4

[0074] Preparation of solid acids b-d:

[0075] The preparation formula of table 1 solid acid b-d

[0076]

[0077] The preparation of solid acid b-d was carried out according to the formula in Table 1 and the operation steps of Example 1.

[0078] Microchannel reactor loaded with solid acid and preparation of hydroxycitronellol:

[0079] Carry out the preparation of loaded microchannel reactor and the preparation of hydroxycitronellol according to the step of embodiment 1, corresponding preparation parameter and reaction result are as shown in table 2 and 3, no by-product rhodamine is produced.

[0080] Table 2 Loaded Microchannel Reactor Preparation Conditions

[0081]

[0082] Table 3 Hydration reaction conditions and results

[0083]

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Abstract

The invention discloses a solid acid, a preparation method thereof, a solid acid-loaded micro-channel reactor, a preparation method of the reactor, and a method for preparing hydroxycitronellal. The solid acid is polystyrene-resin-immobilized N-alkyl amino diphosphoric acid. After the solid acid is immobilized in pore channels of the micro-channel reactor, micro-fiber holes can be formed, the effective contact area of reaction liquid and a catalyst is increased, meanwhile, the use of the micro-channel reactor effectively improves the mass transfer efficiency, and the reaction time is shortenedto several minutes from several hours through the synergistic effect of the reactor and the solid acid. A large amount of inorganic acid such as sulfuric acid and an organic cosolvent are prevented from being used, corrosion to equipment and generation of organic wastewater are greatly reduced, and meanwhile, the problem of catalyst recovery is solved. The generation of a byproduct rose alcohol is avoided, the reaction selectivity is effectively improved, and the aroma quality of the product is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a solid acid and a microchannel reactor carrying the solid acid, and also relates to a method for preparing hydroxycitronellol by citronellol hydration reaction. Background technique [0002] Hydroxycitronellol is an important aroma chemical with a floral aroma, which can be used to prepare floral essences such as cloves and lilies for cosmetics and food flavors. In addition, it is also the main raw material for the preparation of lily of the valley spice hydroxycitronellal. [0003] At present, there are two main catalysts for the hydration reaction of citronellol to prepare hydroxycitronellol, one is inorganic acids such as sulfuric acid, and the other is solid acids such as acidic cation exchange resins. [0004] When utilizing sulfuric acid as the citronellol hydration reaction catalyst, it adopts the mode of batch tank reactor and temperature programming to carry o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J19/00C07C29/04C07C31/20C08F8/40C08F8/32C08F12/08
CPCB01J31/069B01J19/0093C07C29/04C08F8/40C08F8/32C07C31/20C08F12/08
Inventor 车传亮张永振董菁王中华黎源
Owner WANHUA CHEM GRP CO LTD
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