CN209205307U - The equipment of glycerin chlorination production dichlorohydrin - Google Patents

The equipment of glycerin chlorination production dichlorohydrin Download PDF

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Publication number
CN209205307U
CN209205307U CN201822019559.5U CN201822019559U CN209205307U CN 209205307 U CN209205307 U CN 209205307U CN 201822019559 U CN201822019559 U CN 201822019559U CN 209205307 U CN209205307 U CN 209205307U
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China
Prior art keywords
autoclave body
dichlorohydrin
equipment
agitator arm
stirring rod
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CN201822019559.5U
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Inventor
韦兵
张海朋
李建军
杨中原
李萍
林苗苗
王建芹
祝新涛
张瑞
扈世琳
陈凯
黄超鹏
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Shandong MINJI New Material Technology Co.,Ltd.
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SHANDONG MINGJI CHEMICAL CO Ltd
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Abstract

The utility model relates to a kind of equipment for producing dichlorohydrin, and in particular to a kind of equipment of glycerin chlorination production dichlorohydrin.Including reaction kettle autoclave body, in autoclave body over top, motor is set, stirring rod is set on the central axes inside autoclave body, stirring rod is connected to the motor, agitator arm is fixedly mounted in the lower end of stirring rod, it agitator arm and stirring rod inner hollow and communicates, aperture is set on agitator arm, HCl air inlet pipe is set on the stirring rod outside autoclave body, feed pipe is set at the top of autoclave body, in the periphery of autoclave body, temperature-control coating is set, temperature-control coating inner hollow, steam inlet and cooling water outlet is respectively set in the two sides on temperature-control coating top, cooling water inlet and steam gas outlet is respectively set in the two sides of lower part, dichlorohydrin crude product discharge nozzle is arranged in autoclave body bottom.The utility model can make chlorination reaction complete, and side reaction is reduced, and dichlorohydrin quality obtained is high, with high purity, impurity is few, replace mechanical stirring with gas agitating, reduce risk and energy consumption.

Description

The equipment of glycerin chlorination production dichlorohydrin
Technical field
The utility model relates to a kind of equipment for producing dichlorohydrin, and in particular to a kind of glycerin chlorination production dichlorohydrin Equipment.
Background technique
Dichlorohydrin is a kind of chemical reagent, and colourless liquid is micro- to have chloroform smell.As solvent and it is used for organic synthesis. It is not soluble in water, it is dissolved in most organic solvents such as ethyl alcohol, ether.It meets high fever, open fire or is contacted with oxidant, there is the danger for causing burning Danger.Dichlorohydrin is synthesis antiviral drugs " Ganciclovir ", 1,3- dichloroacetone, epoxychloropropane, crosslinking agent, water treatment agent Etc. the raw material of a variety of chemical products.
The production method of industrial dichlorohydrin is mainly using propylene as the propylene high-temperature chloridising and propylene acetate of raw material Method.But the method is all and largely to consume chlorine using propylene as raw material, and waste discharge amount is big.
Production method about dichlorohydrin is also constantly being studied, simple process and using renewable resource glycerol be raw material Glycerol method be concerned.Using glycerol and hydrogen chloride production dichlorohydrin, glycerol hydrochlorination reaction generates 1- chlorine the third two first Alcohol and water, the hydrogen chloride gas being then dissolved in reaction solution are reacted with glycerol and 1- propylene glycol of chlorine again, produce dichlorohydrin.
Existing glycerin chlorination reaction kettle is all made of mechanical stirring, hydrogen chloride is reacted by the mode that bottom is passed through.In the presence of Following disadvantage: (1) hydrogen chloride is passed through by bottom, and under conditions of mechanical stirring, gas is unevenly distributed, and side reaction is more, is caused By-product increases;(2) mechanical agitation process is easily clashed with hydrogen chloride charge air flow, causes stirring chaotic, autoclave It is interior easily to bring danger;(3) mechanical stirring power is big, and energy consumption is higher.
Summary of the invention
In view of the deficiencies of the prior art, setting the purpose of the utility model is to provide a kind of glycerin chlorination production dichlorohydrin Standby, chlorination reaction is complete, and side reaction is few, and dichloropropanol product quality is high, and purity is high, impurity are few, and risk is low, low energy consumption.
The equipment of glycerin chlorination production dichlorohydrin described in the utility model, including reaction kettle autoclave body, at the top of autoclave body Motor is arranged in top, and stirring rod is arranged on the central axes inside autoclave body, and stirring rod is vertically arranged and passes through at the top of autoclave body and electric Machine is connected, and agitator arm, agitator arm and stirring rod inner hollow and phase is fixedly mounted in the lower end of the stirring rod inside autoclave body It is logical, aperture is set on agitator arm, HCl air inlet pipe is set on the stirring rod outside autoclave body, feed pipe is set at the top of autoclave body, Temperature-control coating, temperature-control coating inner hollow are set in the periphery of autoclave body, steam inlet and cold is respectively set in the two sides on temperature-control coating top But cooling water inlet and steam gas outlet is respectively set in water out, the two sides of temperature-control coating lower part, and dichlorohydrin is arranged in autoclave body bottom Crude product discharge nozzle.
Preferably, agitator arm is arranged 4, and agitator arm is uniformly distributed.
Preferably, 6-10 aperture of setting on every agitator arm, preferably 8;Aperture on every agitator arm is inclined Tiltedly setting, each open pore size are 3-5cm, preferably 4cm.By the setting to agitator arm and aperture, so that hydrogen chloride gas It is distributed in reaction kettle more uniform, chlorination reaction is more complete, and side reaction is less, the purity is high of product dichlorohydrin, impurity It is few.
Height of the agitator arm apart from bottom is 1/8th of autoclave body height.
Dichlorohydrin crude product discharge nozzle connects rectification section entrance.
Valve is respectively provided on HCl air inlet pipe, feed pipe and dichlorohydrin crude product discharge nozzle.
Operational process is as follows:
Glycerol, catalyst mixing are added inside autoclave body by feed pipe, the feed liquid liquid level inside autoclave body reaches three/ After at two, steam is passed through by steam inlet and is preheated, after reaching certain temperature, from HCl air inlet pipe to autoclave body inside lead to HCl Gas, each agitator arm of the agitated bar arrival of HCl gas is entered inside autoclave body by aperture again to be reacted, and is stopped in reaction process Only steam heats, and is passed through recirculated water by cooling water inlet and cools down, and controls reactor temperature at 100 DEG C or so, reacts one After the section time, dichlorohydrin crude product is produced by dichlorohydrin crude product discharge nozzle, to the material of dichlorohydrin crude product discharge nozzle extraction It is detected, when wherein dichloropropanol content is greater than 95%, one chloropropyl alcohol less than 1%, is purified into rectification section.
Compared with prior art, the utility model has the advantage that
(1) the utility model can be realized reaction raw materials laterally, it is longitudinal while flowing so that after hydrogen chloride gas entrance It is uniformly distributed in reaction kettle, chlorination reaction is more complete, reduces side reaction, improves dichloropropanol product quality.
(2) it is next to can be avoided the collision belt of agitator arm and hydrogen chloride gas air-flow in mechanical agitation process for the utility model Danger.
(3) the utility model replaces mechanical stirring with gas agitating, reduces risk and energy consumption.
(4) the utility model is by the setting to agitator arm and aperture, so that hydrogen chloride gas is distributed in reaction kettle More uniform, chlorination reaction is more complete, and side reaction is less, and the purity is high of product dichlorohydrin, impurity are few.
(5) it is mentioned by 91.0% to 95.0% or more, one chlorine third using the dichlorohydrin purity of the utility model device preparation Alcohol is down to 1.0% or less by 2.5%.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the equipment of glycerin chlorination production dichlorohydrin described in the utility model;
In figure: 1- motor, 2-HCl air inlet pipe, 3- feed pipe, 4- steam inlet, 5- temperature-control coating, 6- aperture, 7- stirring Impeller, the cooling water inlet 8-, 9- dichlorohydrin crude product discharge nozzle, 10- steam gas outlet, 11- stirring rod, 12- cooling water outlet, 13- autoclave body.
Specific embodiment
The utility model is described further below with reference to embodiment.
Embodiment
A kind of equipment of glycerin chlorination production dichlorohydrin, as shown in Figure 1, including reaction kettle autoclave body 13, on the top of autoclave body 13 Motor 1 is set above portion, stirring rod 11 is set on the central axes inside autoclave body 13, stirring rod 11 is vertically arranged and passes through autoclave body 13 tops are connected with motor 1, and agitator arm 7, agitator arm 7 and stirring is fixedly mounted in the lower end of the stirring rod inside autoclave body 13 It 11 inner hollow of bar and communicates, aperture 6 is set on agitator arm 7, setting HCl air inlet pipe on the stirring rod 11 autoclave body 13 outside 2, feed pipe 3 is set at the top of autoclave body 13, temperature-control coating 5,5 inner hollow of temperature-control coating, on temperature-control coating 5 are set in the periphery of autoclave body 13 Steam inlet 4 and cooling water outlet 12 is respectively set in the two sides in portion, and cooling water inlet is respectively set in the two sides of 5 lower part of temperature-control coating 8 and steam gas outlet 10, dichlorohydrin crude product discharge nozzle 9 is arranged in 13 bottom of autoclave body.
Agitator arm 7 is arranged 4;Agitator arm 7 is uniformly distributed;8 apertures 6 are set on every agitator arm 7;Every is stirred The aperture 6 mixed on impeller 7 is obliquely installed;Each 6 aperture of aperture is 4cm.
Height of the agitator arm 7 apart from bottom is 1/8th of 13 height of autoclave body.
Dichlorohydrin crude product discharge nozzle 9 connects rectification section entrance.
Valve is respectively provided on HCl air inlet pipe 2, feed pipe 3 and dichlorohydrin crude product discharge nozzle 9.
It is specific as follows using the technique of the glycerin chlorination production dichlorohydrin of the equipment:
Glycerol, catalyst mixing are added inside autoclave body 13 by feed pipe 3, the feed liquid liquid level inside autoclave body 13 reaches three After at/bis-, steam is passed through by steam inlet and is preheated, after temperature in the kettle reaches 75 DEG C, from HCl air inlet pipe 2 to autoclave body 13 inside lead to HCl gas, and the agitated bar 11 of HCl gas reaches each agitator arm 7 again by carrying out inside the entrance autoclave body 13 of aperture 6 It reacts, stops steam heating in reaction process, recirculated water is passed through by cooling water inlet 8 and is cooled down, control reactor temperature At 100 DEG C or so, after reacting a period of time, dichlorohydrin crude product is produced by dichlorohydrin crude product discharge nozzle 9, thick to dichlorohydrin The material that product discharge nozzle 9 produces is detected, when wherein dichloropropanol content is greater than 95%, one chloropropyl alcohol less than 1%, into essence Workshop section is evaporated to be purified.

Claims (9)

1. a kind of equipment of glycerin chlorination production dichlorohydrin, it is characterised in that: including reaction kettle autoclave body (13), in autoclave body (13) Motor (1) is arranged in over top, stirring rod (11) is arranged on the internal central axes of autoclave body (13), stirring rod (11) is vertically arranged And pass through and be connected at the top of autoclave body (13) with motor (1), agitator arm is fixedly mounted in the lower end of the internal stirring rod of autoclave body (13) (7), it agitator arm (7) and stirring rod (11) inner hollow and communicates, aperture (6) is set on agitator arm (7), in autoclave body (13) HCl air inlet pipe (2) are set on external stirring rod (11), feed pipe (3) are set at the top of autoclave body (13), in the outer of autoclave body (13) Week setting temperature-control coating (5), temperature-control coating (5) inner hollow, the two sides on temperature-control coating (5) top be respectively set steam inlet (4) and Cooling water inlet (8) and steam gas outlet (10), autoclave body is respectively set in the two sides of cooling water outlet (12), temperature-control coating (5) lower part (13) bottom setting dichlorohydrin crude product discharge nozzle (9).
2. the equipment of glycerin chlorination production dichlorohydrin according to claim 1, it is characterised in that: agitator arm (7) is set Set 4.
3. the equipment of glycerin chlorination production dichlorohydrin according to claim 2, it is characterised in that: agitator arm (7) is equal Cloth distribution.
4. the equipment of glycerin chlorination production dichlorohydrin according to claim 2, it is characterised in that: every agitator arm (7) 6-10 aperture (6) is set on.
5. the equipment of glycerin chlorination production dichlorohydrin according to claim 4, it is characterised in that: each aperture (6) hole Diameter is 3-5cm.
6. the equipment of glycerin chlorination production dichlorohydrin according to claim 4, it is characterised in that: every agitator arm (7) aperture (6) on is obliquely installed.
7. the equipment of glycerin chlorination according to claim 1 production dichlorohydrin, it is characterised in that: agitator arm (7) away from Height from bottom is 1/8th of autoclave body (13) height.
8. the equipment of glycerin chlorination production dichlorohydrin according to claim 1, it is characterised in that: dichlorohydrin crude product goes out Expects pipe (9) connects rectification section entrance.
9. the equipment of glycerin chlorination production dichlorohydrin according to claim 1, it is characterised in that: HCl air inlet pipe (2), Valve is respectively provided on feed pipe (3) and dichlorohydrin crude product discharge nozzle (9).
CN201822019559.5U 2018-12-03 2018-12-03 The equipment of glycerin chlorination production dichlorohydrin Active CN209205307U (en)

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Application Number Priority Date Filing Date Title
CN201822019559.5U CN209205307U (en) 2018-12-03 2018-12-03 The equipment of glycerin chlorination production dichlorohydrin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201822019559.5U CN209205307U (en) 2018-12-03 2018-12-03 The equipment of glycerin chlorination production dichlorohydrin

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111644121A (en) * 2020-06-09 2020-09-11 常州市新鸿医药化工技术有限公司 Hydrogenation dechlorination device and method for trichloroacetone

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111644121A (en) * 2020-06-09 2020-09-11 常州市新鸿医药化工技术有限公司 Hydrogenation dechlorination device and method for trichloroacetone
CN111644121B (en) * 2020-06-09 2022-02-11 常州市新鸿医药化工技术有限公司 Hydrogenation dechlorination device and method for trichloroacetone

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Address after: No.227, Changguo East Road, chemical industry park, Zhangdian District, Zibo City, Shandong Province

Patentee after: Shandong MINJI New Material Technology Co.,Ltd.

Address before: 255000 Shandong city of Zibo province Zhangdian two road Hutian Road on the north side of cross East Chemical Industrial Zone

Patentee before: SHANDONG MINJI CHEMICAL Co.,Ltd.