Method for continuous producing dichlorohydrin and apparatus thereof

A technology of dichloropropanol and chlorination reaction, applied in the introduction of halogen preparation, organic chemistry, etc., can solve the problems of gasification loss, large consumption of HCl gas, long reaction time, etc., achieve easy recycling and reduce waste The amount of production and the effect of reducing waste water production

Active Publication Date: 2009-06-17
CHANG CHUN PLASTICS CO LTD
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Problems solved by technology

The disadvantage of this method is that the reaction time is too long, the consumption of HCl gas is too large and the conversion rate of dichloropropanol is low.
Moreover, the HCl aqueous solution produced after use cannot be recycled and used in the chlorination reaction
[0006] Another method is to use glycerol as a raw material, use aqueous hydrochloric acid as a chlorinating agent, use acetic acid as a catalyst, and use dichloropropanol as a solvent at a reaction temperature of 123 ° C and a reaction pressure of 1 bar (bar). This method has the problem of gasification loss during the reaction due to the hydrochloric acid aqueous solution used, resulting in a low selectivity of glycerol to dichloropropanol, such as 29.7%, so there is a shortcoming that the conversion rate of dichloropropanol is too low

Method used

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  • Method for continuous producing dichlorohydrin and apparatus thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0037] The purpose of this embodiment 1-5 is in order to illustrate the influence of acetic acid concentration on the conversion rate of dichloropropanol, so only illustrate with one chlorination reaction. A 1 liter positive pressure reactor equipped with a stirring device, heating equipment, pressurized lines and components was used. Feed the feed mixture containing glycerol, aqueous hydrochloric acid and acetic acid in the amounts listed in Table 1 below into the above-mentioned reactor, and at a reaction temperature of 145° C. and a reaction pressure of 6 bar, by controlling the feed rate to be 10 ml / Minutes and the control reaction residence time are carried out the first chlorination reaction under the condition of 1.5 hours, observe that acetic acid concentration is compared to dichloropropanol conversion, and experimental result is as shown in table 1.

[0038] Table 1

[0039] Example number 1 2 3 4 5 Glycerin (g) 46 46 46 46 46 Aqueous ...

Embodiment 6-10

[0042]The purpose of this embodiment 6-10 is in order to illustrate the influence of hydrochloric acid aqueous solution concentration on the conversion rate of dichloropropanol, so only illustrate with one chlorination reaction. A 1 liter positive pressure reactor equipped with a stirring device, heating equipment, pressurized lines and components was used. The feed mixture comprising glycerol, aqueous hydrochloric acid solution and acetic acid in the amounts listed in Table 2 below was fed into the above-mentioned reactor, and at the reaction temperature shown in Table 2 and the reaction pressure of 6 bar, by controlling the feed rate to 15 milliliters / minute and control reaction residence time is that under the condition of 1.0 hour, carry out chlorination reaction for the first time, observe the presence of hydrochloric acid aqueous solution and compare dichloropropanol conversion, experimental result is as shown in table 2.

[0043] Table 2

[0044] Example numb...

Embodiment 11

[0048] use figure 1 In the shown reaction device, the hydrochloric acid aqueous solution and the acetic acid that will comprise glycerin, the concentration are 32% by weight respectively with the speed of 1.12 milliliter / minute, 9.71 milliliter / minute and the speed of 0.67 milliliter / minute via the acetic acid feed pipe 4, hydrochloric acid aqueous solution feed Pipe 5 and glycerol feed pipe 6 are fed into the first reactor 1 (capacity is 1 liter), and simultaneously with the same speed of feeding rate, the material is discharged to maintain a fixed liquid level in the reactor (in this embodiment, the output The speed should be 1.12+9.71+0.67 ml / min). The first chlorination reaction was carried out at a reaction temperature of 140° C., a reaction pressure of 6 bar, and a reaction residence time of 1.5 hours. After the reaction, the product is fed into the middle section of the distillation tower 2 through the discharge pipe 7, and the product dichloropropanol is collected fro...

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Abstract

The invention discloses a method for continuously producing dichlorohydrin. The method uses a hydrochloric acid aqueous solution as a chloridizing agent and acetic acid as an accelerant, continuously chloridizes glycerol by controlling the feed speed and the discharge speed to be same, and can obtain the dichlorohydrin with short residence time and high conversion rate. The invention also discloses a device for continuously producing the dichlorohydrin.

Description

technical field [0001] The present invention relates to a method for continuously producing dichloropropanol and its device, in particular to a method for producing dichloropropanol from glycerol with a high conversion rate within a short residence time by controlling the feed rate to be the same as the discharge rate Continuous method for alcohol and device thereof. Background technique [0002] Epichlorohydrin is mainly used in the production of fine chemical products such as epoxy resin and chlorohydrin rubber, which are widely used in the fields of chemical industry, light industry, transportation, medicine, and electronic appliances. [0003] In the past, epichlorohydrin was produced by using propylene as a raw material, chlorinated with chlorine gas as a chlorinating agent, and then epoxidized to obtain epichlorohydrin. However, due to the shortage of oil, the price of propylene will increase day by day, and the by-product glycerol of biodiesel will inevitably be surp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/36C07C29/62
Inventor 黄健富李育贤
Owner CHANG CHUN PLASTICS CO LTD
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