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Method for generating polyvalent alcohol and formiate by extractive crystallization separating cannizzaro process

A technology for extracting crystallization and polyols, applied in chemical instruments and methods, preparation of carboxylate salts, preparation of organic compounds, etc., which can solve problems such as increased equipment investment and operating costs, long production process cycle, and decreased product yield. Achieve the effects of saving equipment investment and dynamic costs, reducing pollution of three wastes, and shortening crystallization cycle

Inactive Publication Date: 2008-03-12
刘荣
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ion exchange resin extraction method requires expensive anion and cation exchange resins; and in the production process, a large amount of acid and alkali are consumed to regenerate the exchange resin, and a large amount of waste liquid is generated to cause environmental pollution; the traditional cooling crystallization method has the following disadvantages: ①Requires low-temperature freezing source, which increases equipment investment and operating costs; ②Because of slow cooling and crystallization, the entire production process cycle is long, which is not conducive to industrial production; Product yield drops

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1: The mixed solution obtained in the above reaction 1 was separated from trimethylolethane and sodium formate in the following steps.

[0044] Step 1: Add n-butanol to the mixed liquid of trimethylolethane and sodium formate, and the volume ratio of the added n-butanol to the mixed liquid of trimethylolethane and sodium formate is 5:1. Make trimethylolethane enter the n-butanol to form the oil phase of the extract, and sodium formate and the raffinate together form the aqueous phase of the extract.

[0045] Step 2: Separate the oil phase and the water phase of the extract,

[0046] Step 3. The aqueous phase of the extract is crystallized by evaporation to obtain 1430 kg of sodium formate crystals.

[0047] Step 4: Add ethyl acetate to the oil phase of the second extract, and the volume ratio of the added ethyl acetate to the oil phase of the second extract is 8:1. The n-butanol in the oil phase is extracted with ethyl acetate, so that trimethylolethane is precipita...

Embodiment 2

[0051] Example 2: The mixed solution obtained in the above reaction 1 was separated from trimethylolethane and sodium formate in the following steps.

[0052] Step 1. Concentrate the mixture of trimethylolethane and sodium formate to make a concentrated solution. The concentration temperature is controlled at 90~100℃, the pressure is controlled at 40~45Kpa, and the concentration of trimethylolethane in the concentrate is controlled at 45% by weight, then n-octanol is added to the concentrated solution, and the volume ratio of the added n-octanol to the concentrated solution is 3:1. Make trimethylolethane enter n-octanol to form the oil phase of the extract, and sodium formate and the raffinate together form the aqueous phase of the extract.

[0053] Step 2: Separate the oil phase and the water phase of the extract,

[0054] Step 3. The aqueous phase of the extract is crystallized by evaporation to obtain 1445 kg of sodium formate crystals.

[0055] Step 4: Add acetone to the oil p...

Embodiment 3

[0059] Example 3: Separating trimethylolpropane and sodium formate from the mixed liquid obtained in the above reaction 2 in the following steps.

[0060] Step 1. Add 2-ethylhexanol to the mixture of trimethylolpropane and sodium formate,

[0061] The volume ratio of the added 2-ethylhexanol to the mixture of trimethylolpropane and sodium formate is 6:1. Make trimethylolpropane into 2-ethylhexanol to form the oil phase of the extract. Sodium formate and the raffinate together form the aqueous phase of the extract.

[0062] Step 2: Separate the oil phase and the water phase of the extract,

[0063] Step 3. The aqueous phase of the extract is crystallized by evaporation to obtain 1138 kg of sodium formate crystals.

[0064] Step 4. Concentrate the oil phase of the extract of step two first, the concentration temperature is controlled at 100-110°C, the pressure is controlled at 1-5Kpa, and the concentration of trimethylolpropane in the concentrate is controlled at 50% by weight. The ...

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PUM

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Abstract

The present invention relates to an extracted, crystalloid and separated Cannizzaros reaction to prepare polyatomic alcohol and formate. The steps are as follows: (1) Solution agent A is added into the mixture liquid between polyatomic alcohol and formate to form an oil phase of the extracting liquid; the formate together with the residual liquid is to form a water-phase of the extracted liquid; (2) the oil phase and the water phase of the extracted liquid are separated; (3) the water phase of the extracted liquid is crystallized and vaporized to obtain formate crystal; (4) the second solution agent B is added into the oil phase of the extracted liquid in step 2 so as to the polyatomic alcohol is separated out with a crystal mode in the mixture agent between A and B; (5) the solid phase of the polyatomic alcohol is separated from the mixture agent between A and B; (6) The mixing agent of A and B is distilled to separate out the solution agent A and the solution agent B; (7) the solid phase of the polyatomic alcohol is dried to recycle the mixing solution agent A and B left in the solid phase of polyatomic alcohol. The present invention is with much lower investment, shorter producing period, simpler operation, much better product quality and higher benefit.

Description

Technical field [0001] The invention relates to a method for separating polyol and formate produced by the Connizaro method by extracting crystallization. It belongs to the field of organic chemicals. Background technique [0002] Polyol products have a wide range of uses: it is an important organic chemical raw material intermediate, which is mainly used in the production of polyurethane foam, alkyd resin coatings and polyester and synthetic lubricants, rosin esters, explosives, surface active The raw materials for the production of chemicals, solvents and plasticizers can also be used as resin diffusing agents, textile solvents, heat stabilizers for polyvinyl chloride resins and the synthesis of various fine chemicals. [0003] At present, the main method for producing polyols such as trimethylolpropane and trimethylolethane is the Connizzaro method. The Connizzaro method is based on the aldol condensation reaction of n-butyraldehyde (propionaldehyde) and aqueous formaldehyde i...

Claims

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Application Information

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IPC IPC(8): C07C29/00C07C31/18C07C53/06C07C51/41
Inventor 刘荣高峰李玉彦
Owner 刘荣