Method for preparing hydroxyacetone by glycerol dehydration

A technology of hydroxyacetone and glycerol, which is applied in the field of preparing hydroxyacetone by dehydration of glycerol, can solve the problem of not preparing simple hydroxyacetone and the like, and achieve the effect of good environmental friendliness

Inactive Publication Date: 2019-04-23
浙江昊唐商业发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no feasible way for the industrial production of hydroxyacetone with simple catalyst preparation, high stability and stable reaction.

Method used

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  • Method for preparing hydroxyacetone by glycerol dehydration

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Dilute sodium metaaluminate, phosphoric acid, 40% silica sol, and distilled water according to n(Al):n(P):n(Si):n(H 2 O) The molar ratio is 1:1:0.1:40 and mixed, stirred for 20 minutes to obtain a gel, and the template agent isopropylamine is added according to the molar ratio n (template agent): n (P) is 2:1, and the stirring is continued until the formation is uniform Gel, put the gel in a reaction kettle, crystallize at 170°C for 1 day; the crystallized product is quenched, filtered, and washed to a pH value of 8, dried at 120°C for 12 hours, and baked in a muffle furnace at 550°C The template agent was removed to obtain the synthetic SAPO-11 molecular sieve.

[0027] 2) The configuration concentration is 12g / L copper bromide salt solution and the concentration is 6g / L chromium chloride salt solution, is dissolved in water with molar ratio 1: 2 and is formulated into mixed solution, adds the SAPO-11 prepared as described in step 1) Molecular sieves, soaked for 24...

Embodiment 2

[0030] 1) Dilute sodium metaaluminate, phosphoric acid, 40% silica sol, and distilled water according to n(Al):n(P):n(Si):n(H 2 O) The molar ratio is 1:1:0.1:40 mixed, stirred for 20 minutes to obtain gel II; the slurry I is added to the gel II, stirred for 30 minutes, according to the molar ratio n (template agent): n (P) is 2:1 Add the template agent isopropylamine, continue to stir until a uniform gel is formed, put the gel into the reaction kettle, and crystallize at 170°C for 1 day. The crystallized product was quenched, filtered, and washed with water until the pH value was 8, dried at 120°C for 12 hours, and calcined in a muffle furnace at 550°C to remove the template agent to obtain SAPO-11 molecular sieve.

[0031] 2) The configuration concentration is 7g / L copper nitrate salt solution and 12g / L chromium nitrate salt solution, dissolved in water at a molar ratio of 1:2 to prepare a mixed solution, adding the SAPO-11 molecular sieve prepared as described in step 1), im...

Embodiment 3

[0034] S1, put glycerin into the preheater and heat to 80°C;

[0035] S2. Import the preheated glycerin into the reactive distillation column, control the vacuum degree in the column at -0.1Mpa, control the temperature of the reboiler at 130°C, and let the glycerin fully contact the catalyst on the surface of the packing layer on the tray for dehydration For the reaction, rectification was carried out with a reflux ratio of 4:1. When the temperature of the overhead distillate reached 120°C, the main product of the 130°C fraction was collected.

[0036] Calculated with the amount of glycerol, the ratio of agent to oil is 0.1%; the reactive distillation rectification column packing is stainless steel corrugated wire mesh and catalyzer; the catalyzer is the prepared loading Cr 2 Cu 2 o 5 / SAPO-11 catalyst.

[0037] The conversion of glycerol and the yield of hydroxyacetone were determined by calibrated GC analysis, and the results are shown in Table 1.

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Abstract

The invention discloses a method for preparing hydroxyacetone by glycerol dehydration. A supported Cr2Cu2O5 / SAPO-11 catalyst is used, SAPO-11 is fully used as a carrier, the prepared supported nano copper chromite catalyst is high in activity and good in stability, a pure glycerol feed can be used for replacing glycerol solution feed, the conversion rate of glycerol is 97% or above, and the selectivity of the hydroxyacetone is 95% or above.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a method for preparing hydroxyacetone by dehydrating glycerin. Background technique [0002] Hydroxyacetone, also known as hydroxyacetone, acetol, acetylmethanol, 1-hydroxy-2-propanone, English name: hydroxyacetone, Hydroxyacetone, 1-hydroxypropan-2-one, Hydroxy-2-propanon, 2-Propanone, 1-hydroxy -, CAS number: 116-09-6, molecular formula: C3H6O2, colorless liquid, freezing point -17°C, boiling point 145-146°C, 96-97°C (20kPa), soluble in water, ethanol, ether. Exist in beer; Tobacco; Honey. The product is unstable, and methanol can be added to stabilize the base. [0003] Hydroxyacetone is mainly used as a raw material for the synthesis of pharmaceutical intermediates 4-methylimidazole, spice 2,3-pentanedione and dye intermediates. It is widely used and in great demand. The current production process mainly uses petrochemical resource 1,2-propanediol as raw material for oxidativ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/52C07C49/17B01J29/85
CPCC07C45/52B01J29/85C07C49/17
Inventor 刘得民
Owner 浙江昊唐商业发展有限公司
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