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A solid acid and its preparation method, a solid acid-loaded microchannel reactor and its preparation method, and a method for preparing hydroxycitronellal

A technology of a microchannel reactor and a solid acid is applied in the field of preparing hydroxycitronellol by hydration reaction of citronellol, which can solve the problems of difficult recovery of catalyst, low reaction conversion rate and yield, influence on product aroma quality, etc. Continuity and operability, improve selectivity, reduce the effect of corrosion of equipment

Active Publication Date: 2022-04-22
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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  • A solid acid and its preparation method, a solid acid-loaded microchannel reactor and its preparation method, and a method for preparing hydroxycitronellal
  • A solid acid and its preparation method, a solid acid-loaded microchannel reactor and its preparation method, and a method for preparing hydroxycitronellal
  • A solid acid and its preparation method, a solid acid-loaded microchannel reactor and its preparation method, and a method for preparing hydroxycitronellal

Examples

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 and a preparation method, a microchannel reactor loaded with solid acid, a preparation method, 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 the pores of the microchannel reactor, microfiber pores will be formed, which increases the effective contact area between the reaction solution and the catalyst. At the same time, the use of the microchannel reactor effectively improves the mass transfer efficiency. The synergy between the two The effect shortens the reaction time from hours to minutes. It avoids the massive use of inorganic acids such as sulfuric acid and organic cosolvents, greatly reduces the corrosion of equipment and the generation of organic waste water, and at the same time solves the problem of catalyst recovery. The generation of the by-product rhodamine is avoided, the selectivity of the reaction 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 Patents(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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