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Dichloropropanol catalyst prepared by glycerol method

A technology of dichloropropanol and catalyst, which is applied in the field of catalysts for preparing dichloropropanol by glycerin method, which can solve the problems of high viscosity of glycerin, high reaction energy consumption, serious environmental pollution, etc., and achieve the improvement of industrial production efficiency and the safety of the use process , the effect of shortening the reaction time

Active Publication Date: 2012-12-05
江苏德纳化学股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the organic nitrile compound catalyst needs to be processed with 30% HCl before use, the reaction process has been increased; secondly, the catalyzer after the HCl treatment contains highly toxic CN in the raffinate after the reaction. - , serious environmental pollution, difficult wastewater treatment
At the same time, these catalysts will still be converted into carboxylic acid catalysts when they encounter acid, so the above-mentioned defects of carboxylic acid catalysts still exist.
[0007] In addition, most of the current glycerol chlorination reactions use reactor-type bubbling reactions with one or more stages in series. Because the reaction is a gas-liquid reaction system, the concentration of HCl in the reaction system is low, and the viscosity of glycerol is high. HCl The reaction between gas and glycerol is not sufficient, and the energy consumption of multi-pot series reaction is high; secondly, the concentration of HCl in the gas-liquid reaction is low, which also causes the yield and selectivity of dichloropropanol to be low, and side effects such as glycerol shrinkage are prone to occur. reaction

Method used

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  • Dichloropropanol catalyst prepared by glycerol method
  • Dichloropropanol catalyst prepared by glycerol method
  • Dichloropropanol catalyst prepared by glycerol method

Examples

Experimental program
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Effect test

Embodiment approach 1

[0023] Embodiment 1 (tank reaction): each example catalyst and proportioning are respectively by 1,2,3,4,7 examples in the attached table.

[0024]Referring to the method described in Chinese patent CN100999443A, add glycerin and a proportioning amount of catalyst into the reactor, start stirring, heat to 110°C, feed anhydrous HCl gas from the bottom of the reactor, and adjust the pressure and flow of HCl gas so that Glycerol is fully reactive. The water generated in the reaction process, unreacted HCl, and part of dichloropropanol are azeotropically distilled from the top of the reactor, and the rest of dichloropropanol and monochloropropanediol flow out from the bottom of the reactor. The reaction ends when no distillate flows out of the condenser. Excess HCl is discharged from the top of the reactor, condensed, dried with concentrated sulfuric acid, and then re-entered into the reactor for recycling after pressurization.

[0025] After the reaction, the still liquid and t...

Embodiment approach 2

[0026] Embodiment 2 (still adds spray reaction): each example catalyzer and proportioning are respectively by appendix 5,6,8.

[0027] see figure 1 , 2 1. Pass glycerin and a proportioned amount of mixed acid catalyst in the head tank E1 into the reaction kettle E3, heat to 65°C, and continuously feed HCl gas from the steel cylinder E2 to E3, and the speed of HCl feeding should not escape. After reacting for 1 hour, the materials were introduced into the reactor E4 to continue chlorination, the reaction temperature was controlled at 90° C., and HCl was continuously introduced to continue the reaction for 1 hour.

[0028] The material after the primary reaction is introduced into the spray reaction tower E8 equipped with corrugated net packing, and the temperature in the tower is controlled at 110°C. HCl is continuously introduced from E7 to the bottom of the spray reaction tower, and the pressure at the outlet of the HCl gas is adjusted to make glycerin The reaction is compl...

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Abstract

The invention relates to epoxy chloropropane intermediate dichloropropanol catalyst prepared by a glycerol method and improvement of a chlorination reaction method. The catalyst is characterized in that the catalyst for reaction is a mixed catalyst of organic carboxylic acid and strong acid, the organic carboxylic acid catalyst is monocarboxylic acid of C1-C12 or dicarboxylic acid of C2-C12, and the dosage is 0.5-5 percent of the content of a glycerol substance; the dosage of the strong acid catalyst is 0.5-15 percent of the content of the glycerol substance; the substance amount ratio of theorganic carboxylic acid to the strong acid is 1:1.0-8.0, and the chlorination reaction is carried out in a reactor and a spray reaction tower with filler, which are connected in series. Compared withsingle catalyst, the invention has high catalytic activity, short reaction time, total reaction time of 6-8 hours and high dichloropropanol yield of larger than 96 percent; particularly, the chlorination reaction is carried out in the reactor and the spray reaction tower with the filler, which are connected in series, and the reaction time can be further shortened by 1-2 hours.

Description

technical field [0001] The invention relates to the improvement of a catalyst for preparing epichlorohydrin intermediate dichloropropanol by a glycerol method and a chlorination reaction method, and in particular relates to a catalyst with high catalytic activity and high reaction yield. Background technique [0002] Epichlorohydrin, also known as epichlorohydrin, is an important organic chemical raw material and fine chemical with a wide range of uses. For example, it is an important raw material for the preparation of epoxy resin, synthetic elastomer, and paper sizing agent. Traditional synthesis methods include propylene high-temperature chlorination method and propylene acetate method, and later developed a glycerin method to prepare epichlorohydrin. The reaction process is as follows: [0003] [0004] The reaction process is divided into two steps, (1) formula; Glycerol chlorination prepares 1,3-dichloropropanol and 1,2-dichloropropanol (because the two are further ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/04B01J27/02B01J27/24B01J27/16B01J27/138B01J27/125C07C29/62C07C31/36
Inventor 秦旭东杨建伟张学君蒋大智段启伟
Owner 江苏德纳化学股份有限公司