CN201272752Y - Apparatus for producing dichlorohydrin by glycerol hydrochlorination - Google Patents
Apparatus for producing dichlorohydrin by glycerol hydrochlorination Download PDFInfo
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- CN201272752Y CN201272752Y CNU2008201511589U CN200820151158U CN201272752Y CN 201272752 Y CN201272752 Y CN 201272752Y CN U2008201511589 U CNU2008201511589 U CN U2008201511589U CN 200820151158 U CN200820151158 U CN 200820151158U CN 201272752 Y CN201272752 Y CN 201272752Y
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Abstract
The utility model relates to a device for preparing dichlorohydrin, which provides a device for preparing dichlorohydrin through hydrochlorinating glycerin. The device comprises an adsorption reaction tower, n stirring tanks, a liquid-phase circulating pump and n gas-phase condensers, wherein a hydrogen chloride gas inlet and a hydrogen chloride liquid-phase outlet are arranged at the bottom of the adsorption reaction tower, and a liquid-phase inlet is arranged on the upper side of the adsorption reaction tower, further, a gas inlet and a reaction liquid outlet are arranged at the bottom of the stirring tank, a reaction liquid inlet and a reaction gas outlet are arranged at the upper portion of the stirring tank, the reaction liquid outlet of the front stirring tank is connected with that of the next reaction liquid, besides, an inlet of the liquid-phase circulating pump is connected with the liquid-phase outlet, the outlet of the liquid-phase circulating pump is connected with the liquid-phase inlet and the reaction liquid inlet of the first stirring tank of the n stirred tanks respectively, and the reaction gas outlet is connected with one of the n gas-phase condensers, wherein the n is an integer ranging from 2 to 10. The utility model has low equipment investment, once-through yield of dichlorohydrin is over 90%, and utilization ratio of hydrogen chloride is over 70%.
Description
Technical field
The utility model relates to the device for preparing dichlorohydrine.
Background technology
At present, the production method of industrial dichlorohydrine, main is the propylene high-temperature chlorination process and the propylene acetate method of raw material with the propylene.
Wherein, 90% above dichlorohydrine intermediate adopts the propylene high-temperature chlorination process to produce in the world.Its technological process mainly comprises propylene high-temperature chlorination system propenyl chloride, two reaction members of propenyl chloride hypochlorination synthesizing dichloropropanol, and reaction formula is:
The characteristics of this processing method are that production process is flexible, technical maturity, and stable operation also can be produced multiple organic synthesis intermediate.But exist equipment corrosion serious, energy consumption is big, chlorine consumption height, and by product is many, and product yield is low, and wastewater flow rate is big, shortcomings such as coke cleaning period weak point.
Propylene acetate method technological process comprises the generation allyl acetate, makes processes such as vinylcarbinol, synthesizing dichloropropanol, and reaction formula is as follows:
Compare with the propylene high-temperature chlorination process, this method has been avoided high-temperature chlorination, and the reaction conditions gentleness is easy to control, noncoking, stable operation, and raw material availability improves greatly, and byproduct of reaction and discharged waste water also significantly reduce.But this method complex process, long flow path, catalyst life is short, and total investment expenses are higher relatively.
More than two kinds of methods all be to be raw material with the propylene, and mass consumption chlorine, the waste water and dregs quantity discharged is big.
Enhancing along with country and environmental protection of enterprise consciousness, the rise of the propylene price that oil shortage causes, just seeking new method in the world wide and substituting original dichlorohydrine production process route, so technology is simple and utilize renewable resources glycerine to rise again for the glycerine method of raw material.
The total reaction equation of preparing dichloropropanol by using glycerol method is as follows:
In fact, this reaction is carried out in two steps, and the first step is that the glycerol hydrochlorination reaction generates 1-propylene glycol of chlorine and water, can generate a spot of 2-propylene glycol of chlorine simultaneously, this two kind of glycerin chlorohydrin continues hydrochlorinate generation 1,1 of 3-two chloro-2-propyl alcohol and minute quantity, 2-two chloro-3-propyl alcohol then.Concrete response situation is as follows:
The method that patent US2144612 introduces is that adding is a kind of water insoluble in reaction system, but can dissolve the solvent of dichlorohydrine, for example n-butyl ether, amyl ether, dichloropropylene, chlorobenzene, orthodichlorobenzene etc.Temperature is controlled under the azeotropic point of reaction mixture carries out, and the reaction times is 30～40 hours, and the dichlorohydrine molar yield is the highest can to reach 91%.This method helps continuous dewatered characteristics in distillation in the preparation of dichlorohydrine, and can reduce the generation of condenses to greatest extent, therefore the selectivity height of reaction.But concentration of reactants has been diluted in the existence of organic solvent greatly, causes the reaction times longer, increases energy consumption, reduce usage ratio of equipment, and, can cause the increase of later separation burden behind the plus solvent from industrialized angle, therefore be difficult to realize industrialization.
Patent CN100999442A discloses a kind of continuous processing, glycerine enters in single or a plurality of reactors as the catalyzer adverse current with carboxylic acid and carries out, and reactant enters rectifying tower continuously, adopts component distillation to remove the water and the dichlorohydrine of generation, promote reaction forward to carry out the tower bottoms circulating reaction.Because the countercurrent flow of gas liquid reaction thing, so the hydrogenchloride utilization ratio improves.In addition, adopt not volatile catalyzer, so catalyst levels is little, but this process energy consumption is higher, plant factor is lower.
The method that patent CN101182283A introduces is that glycerine is added injection-type reactor with catalyzer, the liquid phase recycle pump is extracted glycerine and catalyzer out in injection-type reactor, enter injection-type reactor from the injection-type reactor top with spray regime again, sucking hydrogen chloride gas from the injection-type reactor sidepiece fully reacts with liquid phase material reactor, spray the negative pressure that produces simultaneously and will react the water that generates, the form with azeotrope of dichlorohydrine and hydrogenchloride is taken out of, through condenser with the water in the azeotrope and the dichlorohydrine condensation product the most that gets off, and the unreacted hydrogen chloride gas circulation is utilized, this technology has the raw material availability height, the characteristics that speed of reaction is fast, but equipment is comparatively complicated, not easy to operate.
In a word, the existing device that is used to prepare dichlorohydrine, product yield is low, and equipment is comparatively complicated, and investment is big, is difficult for suitability for industrialized production.
Summary of the invention
The utility model purpose provides a kind of device of preparing dichlorohydrin by glycerol hydrochlorination, to overcome some shortcomings of existing technology.
The device of preparing dichlorohydrin by glycerol hydrochlorination of the present utility model comprises absorption reaction tower, a n stirring tank, liquid phase recycle pump and n gas phase condenser;
The bottom of described absorption reaction tower is provided with the gas inlet and the liquid phase outlet of hydrogenchloride, and top is provided with the liquid phase inlet;
The bottom of described stirring tank is provided with gas inlet and reaction liquid outlet, and top is provided with reaction liquid inlet and reaction gas outlet, and the reaction liquid outlet of previous stirring tank is connected with the reaction liquid inlet of a back stirring tank;
The inlet of described liquid phase recycle pump is connected with described liquid phase outlet by pipeline, the liquid phase outlet of circulating pump respectively with liquid phase inlet and n stirring tank in the reaction liquid of first stirring tank enter the mouth and be connected, one in reaction gas outlet and n the gas phase condenser is connected;
N is 2～10 integer.
The utility model is operation like this:
At first catalyzer is mixed with the glycerine raw material, obtain stock liquid, then described stock liquid is sent into the absorption reaction tower from the liquid phase inlet, simultaneously, the gas that will contain hydrogenchloride is sent into the absorption reaction tower from the gas inlet, stock liquid and hydrogenchloride is the counter current contact reaction in the absorption reaction tower, and partly sends the material of absorption reaction tower bottom back to the absorption reaction tower by the liquid phase recycle pump, and part branches to first stirring tank in n the stirring tank;
The gas phase mixture that steams from the stirring tank top, one that enters respectively in n the gas phase condenser is carried out gas-liquid separation, isolated hydrogen chloride gas, send back to and enter the absorption reaction tower, isolated phlegma, be gaseous products, the mother liquor from coming out in n (being last) stirring tank bottom is liquid-phase product;
The utility model is according to the suitable operational path of characteristics design of glycerol hydrochlorination reaction different steps, facility investment is little, operation control is simple, the speed of reaction height, be easy to amplify and produce, the once through yield of dichlorohydrine reaches more than 90%, and hydrogenchloride has obtained utilizing to greatest extent, and its utilization ratio reaches more than 70%.
Description of drawings
Fig. 1 is the apparatus structure synoptic diagram.
Embodiment
Referring to Fig. 1, the device of preparing dichlorohydrin by glycerol hydrochlorination of the present utility model comprises absorption reaction tower 1, a n stirring tank 2, liquid phase recycle pump 3 and n gas phase condenser 4;
The bottom of described absorption reaction tower 1 is provided with the gas inlet 103 and the liquid phase outlet 101 of hydrogenchloride, and top is provided with liquid phase inlet 102;
The bottom of described stirring tank 2 is provided with gas inlet 201 and reaction liquid outlet 202, top is provided with reaction liquid inlet 203 and reaction gas outlet 204, and the reaction liquid outlet 202 of previous stirring tank 2 is connected with the reaction liquid inlet 203 of a back stirring tank 2;
The inlet of described liquid phase recycle pump 3 is connected with described liquid phase outlet 101 by pipeline, the outlet of liquid phase recycle pump 3 respectively with liquid phase inlet 102 and n stirring tank 2 in the reaction liquid of first stirring tank 201 enter the mouth and 203 be connected, one in reaction gas outlet 204 and n the gas phase condenser 4 is connected;
N is 2～10 integer.
Preferably, n is 3～5 integer.
Claims (2)
1. the device of preparing dichlorohydrin by glycerol hydrochlorination is characterized in that, comprises absorption reaction tower (1), a n stirring tank (2), liquid phase recycle pump (3) and n gas phase condenser (4);
The bottom of described absorption reaction tower (1) is provided with the gas inlet (103) and the liquid phase outlet (101) of hydrogenchloride, and top is provided with liquid phase inlet (102);
The bottom of described stirring tank (2) is provided with gas inlet (201) and reaction liquid outlet (202), top is provided with reaction liquid inlet (203) and reaction gas outlet (204), and the reaction liquid outlet (202) of previous stirring tank (2) is connected with the reaction liquid inlet (203) of a back stirring tank (2);
The inlet of described liquid phase recycle pump (3) exports (101) by pipeline and described liquid phase and is connected, the outlet of liquid phase recycle pump (3) respectively with liquid phase inlet (102) and n stirring tank (2) in the reaction liquid of first stirring tank (201) enter the mouth (203) be connected, one in reaction gas outlet (204) and n the gas phase condenser 4 is connected;
N is 2～10 integer.
2. the device of preparing dichlorohydrin by glycerol hydrochlorination according to claim 1 is characterized in that, n is 3～5 integer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2008201511589U CN201272752Y (en) | 2008-07-24 | 2008-07-24 | Apparatus for producing dichlorohydrin by glycerol hydrochlorination |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2008201511589U CN201272752Y (en) | 2008-07-24 | 2008-07-24 | Apparatus for producing dichlorohydrin by glycerol hydrochlorination |
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| CN201272752Y true CN201272752Y (en) | 2009-07-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNU2008201511589U Expired - Lifetime CN201272752Y (en) | 2008-07-24 | 2008-07-24 | Apparatus for producing dichlorohydrin by glycerol hydrochlorination |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104415645A (en) * | 2013-08-31 | 2015-03-18 | 福建豪邦化工有限公司 | System for preparing dichloropropanol |
-
2008
- 2008-07-24 CN CNU2008201511589U patent/CN201272752Y/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104415645A (en) * | 2013-08-31 | 2015-03-18 | 福建豪邦化工有限公司 | System for preparing dichloropropanol |
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Granted publication date: 20090715 |
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| CX01 | Expiry of patent term |