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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., 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 three waste pollution, and shortening the crystallization cycle

Inactive Publication Date: 2010-08-25
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 solution of trimethylolethane and sodium formate, and the volume ratio of the added n-butanol to the mixed solution of trimethylolethane and sodium formate is 5:1. Make trimethylolethane into n-butanol to form the oil phase of the extract, sodium formate and the raffinate together form the water phase of the extract,

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

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

[0047] Step 4: Add ethyl acetate to the oil phase of the extract in step 2, and the volume ratio of the added ethyl acetate to the oil phase of the extract in step 2 is 8:1. Utilize ethyl acetate to extract n-butanol in the oil phase, trimethylolethane is separated out wi...

Embodiment 2

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

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

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

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

[0055] Step 4, adding acetone...

Embodiment 3

[0059] Embodiment 3: The mixed solution obtained in the above reaction 2 is separated from trimethylolpropane and sodium formate in the following steps.

[0060] Step 1, add 2-ethylhexanol in the mixed solution of trimethylolpropane and sodium formate,

[0061] The volume ratio of the mixed solution of the added 2-ethylhexanol to 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 water phase of the extract,

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

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

[0064] Step 4. Concentrate the oil phase of the extract in step 2. The concentration temperature is controlled at 100-110°C, the pressure is controlled at 1-5Kpa, and the concentration of trimethylolpropane in the concentrated solution is control...

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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 polyalcohol and formate formed by the Connizzaro method by extractive crystallization. It belongs to the field of organic chemical industry. Background technique [0002] Polyol products have a wide range of uses: they are an important class of organic chemical raw material intermediates, which are mainly used in the production of polyurethane foams, alkyd resin coatings and polyesters, as well as in the synthesis of lubricants, rosin esters, explosives, surface active It can also be used as the raw material for the production of solvents, solvents and plasticizers. It can also be used as a diffusion agent for resins, a textile solvent, a heat stabilizer for polyvinyl chloride resins, and the synthesis of various fine chemicals. [0003] At present, the methods for producing polyols such as trimethylolpropane and trimethylolethane mainly include the Connizzaro method. The Connizzaro method is an aldol ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/00C07C51/41C07C31/18C07C53/06
Inventor 刘荣高峰李玉彦
Owner 刘荣
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