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Technology for preparing sodium dehydroacetate in membrane reactor with immobilized catalyst

A technology of sodium dehydroacetate and membrane reactor, which is applied in the field of preparation technology of sodium dehydroacetate, can solve the problems of difficult separation of by-products of diketene polymerization, unrecoverable catalyst, etc., and achieves high catalytic activity, reaction selectivity, and mechanical strength. High, improve the effect of reaction yield

Active Publication Date: 2018-05-04
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] Therefore, in view of the unrecoverable catalyst in the production process of sodium dehydroacetate, the diketene polymerization by-products are difficult to separate and other problems, the technical problem to be solved in the present invention is to develop a preparation method that adopts a reusable catalyst and is easy to separate the diketene polymerization by-products. Sodium dehydroacetate process

Method used

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  • Technology for preparing sodium dehydroacetate in membrane reactor with immobilized catalyst
  • Technology for preparing sodium dehydroacetate in membrane reactor with immobilized catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0037] 1) First, toluene is injected into the ceramic membrane reactor equipped with a solid-supported catalyst, the circulation pump is turned on, and then the diketene feeding pump is turned on, and the diketene feeding pump is turned on within 0.5h. The feed mass ratio of diketene and toluene is 1:5 The reaction temperature is controlled to 50°C, the reactor pressure is controlled to 0.8MPa, and the catalyst addition amount is 0.5wt% of the total feed amount (the total mass of the mixed solution of the catalyst, diketene and toluene). The ceramic nanofiltration membrane is made of Al 2 O 3 With TiO 2 Manufactured, the membrane pore size is 1~2nm;

[0038] 2) The solid supported catalyst KOH-NaOH / Al described in step 1 2 O 3 It is prepared by dipping method, KOH-NaOH is used as the active component, the mass ratio of KOH to NaOH is 1:1, the active component is weighed and prepared into a 20wt% aqueous solution, the carrier is Al2O3, the particle size is 100 mesh, and the active ...

Embodiment 2

[0041] 1) First, toluene is injected into the ceramic membrane reactor equipped with a solid-supported catalyst, the circulation pump is turned on, and then the diketene feeding pump is turned on, and the diketene feeding pump is turned on within 1 hour. The feed mass ratio of diketene and toluene is 1:10. The reaction temperature is controlled at 60°C, the reactor pressure is controlled at 1 MPa, and the catalyst addition amount is 0.5 wt% of the total feed amount (the total mass of the mixed solution of the catalyst, diketene and toluene). The ceramic nanofiltration membrane is made of Al 2 O 3 With TiO 2 Manufactured, the membrane pore size is 1~2nm;

[0042] 2) The supported catalyst KOH-NaOH / SiO as described in step 1 2 Prepared by dipping method, with KOH-NaOH as the active component, the mass ratio of KOH to NaOH is 2:1, weigh the active component and prepare a 25wt% aqueous solution, the carrier is SiO 2 , The particle size is 200 meshes, the active component accounts for ...

Embodiment 3

[0045] 1) First, toluene is injected into the ceramic membrane reactor equipped with a solid-supported catalyst, the circulation pump is turned on, and then the diketene feeding pump is turned on, and the diketene feeding pump is turned on within 1 hour. The feed mass ratio of diketene and toluene is 1:15. The reaction temperature is controlled at 70°C, the reactor pressure is controlled at 2MPa, and the catalyst addition amount is 3wt% of the total feed amount (the total mass of the mixed solution of the catalyst, diketene and toluene). The ceramic nanofiltration membrane is made of Al 2 O 3 With TiO 2 Manufactured, the membrane pore size is 1~2nm;

[0046] 2) The solid-supported catalyst KOH-NaOH / ZSM-5 described in step 1 is prepared by an impregnation method, with KOH-NaOH as the active component, and the mass ratio of KOH to NaOH is 3:1. Weigh the active component and prepare 30wt% aqueous solution, the carrier is ZSM-5, the particle size is 300 mesh, the ratio of the active ...

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Abstract

The invention discloses a technology for preparing sodium dehydroacetate in a membrane reactor with an immobilized catalyst. The technology comprises the following steps: firstly, pumping methylbenzene into the ceramic membrane reactor filled with the immobilized catalyst, adding ketene dimmer within 0.5 to 1 h, enabling the feeing mass ratio of ketene dimmer to methylbenzene to be 1:(5 to 15), controlling the reaction temperature to be 50 to 70 DEG C, and controlling the pressure of the reactor to be 0.8 to 2 MPa, wherein the addition quantity of the catalyst is 0.5wt% to 3wt% of total feeding quantity, the immobilized catalyst is prepared with an impregnation method; when the HPLC content of ketene dimmer in the reaction solution is greater than or equal to 0.5%, after a polymerization reaction ends, enabling a penetrating fluid to enter into a sodium hydroxide water solution used for an extraction tower for carrying out an extraction reaction according to the mole ratio of ketene dimmer to sodium hydroxide being 1:(1 to 1.5), concentrating a sodium dehydroacetate solution, and carrying out drying, smashing and product packaging at the temperature of 90 to 105 DEG C, wherein theyield of the prepared sodium dehydroacetate is greater than or equal to 99%, and the product content is greater than or equal to 99.8%. According to the technology, the production cost is effectivelyreduced, the quantity of three wastes during production is reduced, and the prepared sodium dehydroacetate is high in yield.

Description

Technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a preparation process of sodium dehydroacetate. Background technique [0002] Sodium dehydroacetate [0003] Appearance properties: white crystalline powder. [0004] Solubility: soluble in water (33g / 100g at 25°C), but hardly soluble in organic solvents such as ethanol. [0005] Molecular weight: 191.1 [0006] Melting point: 110°C [0007] use: [0008] Food preservatives, preservatives. This product has a strong antibacterial effect on yeasts, spoilage bacteria, and molds in food. It is widely used in the preservation and preservation of meat, fish, vegetables, fruits, beverages, cakes, etc. Spectrum bacteriostatic agent. [0009] Existing technology synthesis process: [0010] At present, the conventional industrial production method is: diketene is condensed in the solvent toluene under the action of the catalyst triethylenediamine and catechol to produce dehydroacetic acid,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D309/36B01J23/04B01J29/40B01J37/02B01J37/08B01J8/00
CPCB01J8/006B01J23/04B01J29/40B01J37/0201B01J37/08B01J2229/18C07D309/36
Inventor 庆九俞新南刘芳朱小刚
Owner NANTONG ACETIC ACID CHEM
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