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Process for preparing alpha-acetyl-gamma-butyrolactone for co-production of various phosphates

A technology of butyrolactone and acetyl, which is applied in the field of co-production of various phosphates while preparing α-acetyl-γ-butyrolactone, so as to avoid environmental pollution, reduce production cost and improve the conditions of comprehensive utilization Effect

Inactive Publication Date: 2012-08-01
SHANXI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the method of producing α-acetyl-γ-butyrolactone and co-producing various phosphates has not been reported in relevant literature at home and abroad.

Method used

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  • Process for preparing alpha-acetyl-gamma-butyrolactone for co-production of various phosphates
  • Process for preparing alpha-acetyl-gamma-butyrolactone for co-production of various phosphates
  • Process for preparing alpha-acetyl-gamma-butyrolactone for co-production of various phosphates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Preparation of α-acetyl-γ-butyrolactone: Add 11.70g γ-butyrolactone, 17.90g ethyl acetate Ester and catalyst metal sodium 3.43g, carry out acylation, then lower the temperature, when the temperature drops to 62°C, add 26.95g of 51% phosphoric acid solution dropwise under stirring, after the addition, fully stir, let stand to separate layers, The aqueous phase was separated over time. The organic phase was rectified (vacuum degree: 0.08Mp) to obtain 15.90 g of α-acetyl-γ-butyrolactone with a purity of 99.1%.

[0019] 2) Preparation of sodium dihydrogen phosphate: adjust the pH value of the water phase to 3.0 with 51% phosphoric acid, concentrate, cool down to room temperature, filter under reduced pressure to obtain 2110 g of sodium dihydrogen phosphate dihydrate, and continue to dehydrate at a constant temperature of 120 ° C for 30 minutes to obtain no Sodium dihydrogen phosphate water 16.23g, product analysis index and industrial sodium dihydrogen phosphate standar...

Embodiment 2

[0023] 1) Preparation of α-acetyl-γ-butyrolactone: the oil-water separation temperature was 61° C., and the rest were the same as in Example 1 to obtain 15.66 g of α-acetyl-γ-butyrolactone with a purity of 99.3%.

[0024] 2) Preparation of sodium hexametaphosphate: the aqueous phase was adjusted to pH 2.8 with 51% phosphoric acid, concentrated, cooled to room temperature, filtered under reduced pressure to obtain 20.60 g of sodium dihydrogen phosphate dihydrate, and dehydrated at 120° C. for 30 minutes to obtain no Sodium dihydrogen phosphate in water, then polymerize it at a constant temperature at 700°C for 30 minutes, then pour the molten liquid into an iron container cooled by a water bath, cool to room temperature, crush it with a pulverizer, and pass through a 35-mesh sieve , to get 12.61g sodium hexametaphosphate. The product analysis results and the indicators of sodium hexametaphosphate standard HG / T2519-2007 are listed in Table 2. The sodium hexametaphosphate prepar...

Embodiment 3

[0029] 1) The preparation of α-acetyl-γ-butyrolactone is the same as in Example 1.

[0030] 2) Preparation of sodium trimetaphosphate: adjust the pH value of the water phase to 3.0 with 51% phosphoric acid, concentrate, cool down to room temperature, filter under reduced pressure to obtain 2110 g of sodium dihydrogen phosphate dihydrate, and continue to dehydrate at 120°C for 30 minutes to obtain anhydrous 16.23 g of sodium dihydrogen phosphate, then polymerized at a constant temperature of 550°C for 5 hours, then cooled to room temperature, crushed with a pulverizer, and passed through a 35-mesh sieve to obtain 12.70 g of sodium trimetaphosphate. The content determination of sodium trimetaphosphate is carried out by the method of "research on the content determination method of industrial grade sodium trimetaphosphate", and the index of the product is shown in Table 3.

[0031] The sodium trimetaphosphate index produced by the present invention of table 3

[0032] p...

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Abstract

The invention provides a process for preparing alpha-acetyl-gamma-butyrolactone for co-production of various phosphates. The process is applicable to producing the alpha-acetyl-gamma-butyrolactone through acylation and phosphoric acid neutralization of gamma-butyrolactone and acetyl reagents serving as raw materials under the catalytic action of metallic sodium, and effective separation of an organic phase and an aqueous phase is achieved through controlling the concentration of phosphoric acid and the system temperature during oil-water separation. The organic phase is rectified to obtain alpha-acetyl-gamma-butyrolactone; and sodium dihydrogen phosphate dihydrate, sodium hexametaphosphate, sodium trimetaphosphate, sodium acid pyrophosphate, sodium dihydrogen phosphate dodecahydrate, trisodium phosphate dodecahydrate, sodium tripolyphosphate and sodium pyrophosphate are obtained through steps such as pH adjustment, concentration, decompressional filtration and the like of the aqueous phase. The process produces both main products and byproducts, achieves co-production of various products by one process, energy conservation, emission reduction and ecological environment protection, and is safe in operation, simple in process, easy to industrialize and low in cost.

Description

technical field [0001] The invention relates to a method for preparing a pharmaceutical intermediate and various alkali metal phosphates, in particular to a method for preparing α-acetyl-γ-butyrolactone and co-producing various phosphates simultaneously. Background technique [0002] α-acetyl-γ-butyrolactone is an important organic chemical raw material and pharmaceutical intermediate. And, with the downstream products of α-acetyl-γ-butyrolactone (vitamin B 1 , Cyclopropylamine, etc.) The increase in the development and application of α-acetyl-γ-butyrolactone has continuously increased the demand. The production process of this product will generate a large amount of phosphate wastewater solution. Phosphate is an important chemical raw material, which has a wide range of uses in washing, water treatment, food industry, oil drilling, mineral processing, metallurgy, metal anticorrosion, color film washing, printing, fiber and paper industry, etc. In recent years, with With ...

Claims

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Application Information

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IPC IPC(8): C07D307/33C01B25/30C01B25/445C01B25/42C01B25/41
Inventor 李美萍王伟冯彦琳祁成福付晋平胡永钢张生万
Owner SHANXI UNIV
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