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CN103724158B - A kind of process units of chloropropene - Google Patents

A kind of process units of chloropropene Download PDF

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Publication number
CN103724158B
CN103724158B CN201310699185.5A CN201310699185A CN103724158B CN 103724158 B CN103724158 B CN 103724158B CN 201310699185 A CN201310699185 A CN 201310699185A CN 103724158 B CN103724158 B CN 103724158B
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propylene
tank
tower
chloropropene
chloride
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CN103724158A (en
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薄纯金
王吉峰
李胜军
宋朋斌
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SHANDONG HAIYI CHEMICAL TECHNOLOGY Co Ltd
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SHANDONG HAIYI CHEMICAL TECHNOLOGY Co Ltd
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Abstract

The invention belongs to chemical field, be specifically related to the process units of a kind of chloropropene.The process units of chloropropene of the present invention includes following structure: propylene tank is parallel with dehydrator and dry propylene tank by pipeline, dry propylene tank is in series with propylene subcooler, the other end of propylene subcooler is parallel with condensation and steams tower and chloride cooler, condensation steams tower and chloride cooler is in series with steamer, and the other end of steamer has been sequentially connected in series propylene surge tank, heat exchanger and chloride reactor;The other end of chloride reactor has been sequentially connected in series chlorine evaporimeter and Chlorine Buffer Vessel.The beneficial effects of the present invention is, use the chloropropene for preparing of assembly of the invention, its yield brings up to 80 85% from the 75 of conventional method 80%, and it is less to use assembly of the invention to carry out reacting its side reaction, and production efficiency is high.

Description

A kind of process units of chloropropene
Technical field
The invention belongs to chemical field, be specifically related to the process units of a kind of chloropropene.
Background technology
The physical property of chloropropene is: colourless flammable liquid, is corrosive and excitant odor.It is slightly soluble in water, with second Alcohol, chloroform, ether and petroleum ether are miscible.Its purposes: can as producing the intermediate of epoxychloropropane, propenyl, glycerine etc., As the solvent of special reaction, it also it is the raw material of agricultural chemicals, medicine, spices, coating.For organic synthesis and pharmaceuticals industry, 3-chlorine Propylene has another name called allyl chloride, is a kind of organic synthesis raw material, on agricultural chemicals in synthetic insecticide list, dimehypo and cartap Mesosome N, N-dimethyl propylene amine and pyrethroid intermediate propylene alcohol ketone, be the most also medicine, synthetic resin, coating, perfume (or spice) The important source material of material etc..These product have the reactivity of alkene and halogenated hydrocarbons concurrently, are the organic of glycerine, epoxychloropropane, propenyl etc. Synthetic intermediate.It is also used for agricultural chemicals, the raw material of medicine.Also act as synthetic resin, coating, binding agent, plasticizer, stabilizer, The raw material of the fine chemicals such as surfactant, lubricant, soil conditioner, spices, mainly for the manufacture of epoxychloropropane, sweet Oil, chloropropyl alcohol, propenyl, agricultural insecticide are double, medicine, resin, coating, adhesive, and sodium allylsulfonate, lubricant etc..With In organic synthesis, agricultural chemicals, coating, synthetic resin, also serve as adhesive, lubricant etc.
The production method of chloropropene has the most several:
(1) high-temperature chlorination
Prepared by propylene high-temperatureization.Reaction equation: CH3CH=CH2+Cl2→ClCH2CH=CH2+HCl
By dry propylene through 350~400 DEG C of preheatings, the heated gasification of liquid chlorine, two kinds of materials are under high velocity jet state Mixing and react, propylene is 4~5: 1 (mol ratios) with the proportioning of chlorine, reactor residence time 1.5~2s, reaction temperature Spend 470~500 DEG C.Product be chilled to 50~100 DEG C to remove HCl and propylene, then be fractionated into i.e. obtaining product.This method is Domestic and international most of manufacturing enterprise is used.
(2) propylene process for oxychlorination
The propylene, hydrogen chloride and the oxygen that mix in 2.5~(1: 1: 1)~0.2 (mol ratio) ratio are anti-at fluid bed Answering in device and react, selecting catalyst is Te, the V being loaded on carrier2O5Or H3PO4, and add nitrogenous thing and make accelerator, Carry out normobaric oxygen chlorination reaction in 240~260 DEG C, prepare chlorallylene.Reaction equation: CH3CH=CH2+HCl+1/2O2[urge Agent] → CH2=CHCH2Cl+H2O
(3) allyl alcohol chloridising
Reaction equation: CH2=CHCH2OH[CuCl2, HCl] and → CH2=CHCH2Cl+H2O
In 10~20 DEG C, sulfuric acid is instilled in allyl alcohol, stannous chloride and hydrochloric acid, insulation reaction 5h after dropping, stand Layering, upper liquid water, 5% sodium carbonate liquor, water are respectively washed 1 time, after point most water, distillation more than 40 DEG C cuts of collection, it is 3-chlorine Propylene.This method is applicable to small lot batch manufacture.
Therefore need to design, for above-mentioned method, the chloropropene process units that a kind of yield high efficiency is high.
Summary of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of yield high efficiency height and the chloropropene of simple in construction Process units.
The chloropropene process units of the present invention is to solve above technical problem by following technical scheme:
The process units of chloropropene, this device includes following structure:
Described propylene tank is parallel with dehydrator and dry propylene tank 3 by pipeline, and raw material propylene is sent into the propylene of tank field Whether tank stores, need dehydration to enter back into dry propylene tank 3 according to the moisture content of propylene;
Described dry propylene tank 3 is in series with propylene subcooler, and the other end of described propylene subcooler is parallel with condensation and steams Going out tower and chloride cooler, described condensation steams tower and chloride cooler is in series with steamer, another of steamer End has been sequentially connected in series propylene surge tank, heat exchanger and chloride reactor;
Raw material propylene and the Propylene recovery in dry propylene tank 3 divide two-way, and described raw material propylene and Propylene recovery are at propylene After the mutual heat exchange of subcooler, a road flow to condensation steam column overhead spray refrigeration, another road through perchlorhydria cooler to entrance Condensation steams the reaction mass cooling of tower, and makes entrance steamer after self vaporization, enters propylene surge tank after completely vaporizing;
The other end of described chloride reactor has been sequentially connected in series chlorine evaporimeter and Chlorine Buffer Vessel, and liquid chlorine is through chlorine Chlorine Buffer Vessel is entered, by delivering to the mixing section of chlorination reactor after metering after evaporimeter gasification;
The described propylene after vaporization enters heat exchanger after metering, will by chlorination reactor reaction mass out Propylene after vaporization is preheated to 360 DEG C and enters chlorination reactor mixing section, and propylene uniformly mixes with the mol ratio of 4-6:1 with chlorine Rear entrance reactor carries out high-temperature chlorination;
Reaction product include chloropropene, 1,2-dichloropropane+1,3-dichloropropylene, the propylene of excess, hydrogen chloride mixed Close gas;
The thick chloropropene of reaction product material and hydrogen chloride pass through and propylene heat exchange, and reaction propylene is preheated to uniform temperature, Reaction mass steams the propylene heat exchange of column overhead again with condensation, then cools down to chloride cooler through liquid reactions propylene, cold But enter condensation to about-10 DEG C and steam tower;
Thick chloropropene and HCl separation in condensation steams tower, hydrogen chloride becomes hydrochloric acid through absorption, and propylene is through overvoltage It is recycled to propylene tank after contracting, recycles;
Thick chloride squeezes into tank field semi-finished product tank through pump, in rectifying column rectifying and purification, obtains finished product chloropropene.
The production process of chloropropene includes following step:
Liquid chlorine enters Chlorine Buffer Vessel after chlorine evaporimeter gasifies, by delivering to the mixing of chlorination reactor after metering Section;
Whether the propylene tank that raw material propylene is sent into tank field stores, need dehydration to enter back into dry propylene according to the moisture content of propylene Tank 3;Then divide two-way with the Propylene recovery in dry propylene tank 3, described raw material propylene and Propylene recovery are in propylene subcooler phase Mutually after heat exchange, a road flows to condensation and steams column overhead spray refrigeration, and another road steams entering condensation through perchlorhydria cooler The reaction mass cooling of tower, and make entrance steamer after self vaporization, enter propylene surge tank after completely vaporizing;
The described propylene after vaporization enters heat exchanger after metering, will by chlorination reactor reaction mass out Propylene after vaporization is preheated to 360 DEG C and enters chlorination reactor mixing section, and propylene uniformly mixes with the mol ratio of 4-6:1 with chlorine Rear entrance reactor carries out high-temperature chlorination;
Reaction product include chloropropene, 1,2-dichloropropane+1,3-dichloropropylene, the propylene of excess, hydrogen chloride mixed Close gas;
The thick chloropropene of reaction product material and hydrogen chloride pass through and propylene heat exchange, and reaction propylene is preheated to uniform temperature, Reaction mass steams the propylene heat exchange of column overhead again with condensation, then cools down to chloride cooler through liquid reactions propylene, cold But enter condensation to about-10 DEG C and steam tower;
Thick chloropropene and HCl separation in condensation steams tower, hydrogen chloride becomes hydrochloric acid through absorption, and propylene is through overvoltage It is recycled to propylene tank after contracting, recycles;
Thick chloride squeezes into tank field semi-finished product tank through pump, in rectifying column rectifying and purification, obtains finished product chloropropene;
Described reaction equation is:
CH3-CH=CH2+Cl2 CH2Cl-CH=CH2 + HCl
CH3-CH=CH2+Cl2 CH3-CHCl-CH2Cl
CH2Cl-CH=CH2+Cl2 CH2Cl-CH=CHCl+HCl
CH3-CH2-CH3+Cl2 CH3-CH2-CH2Cl+HCl
CH3CH=CH2+3Cl2 3C+6HCl。
Propylene is 5:1 with the mol ratio of chlorine.
When its moisture content of raw material propylene is less than or equal to 10ppm, propylene is directly entered dry propylene tank 3;
When its moisture content of raw material propylene is more than 10ppm, by raw material propylene dehydration to its moisture content less than or equal to 10ppm Rear feeding dry propylene tank 3.
The step that thick chloride refines as finished product chloropropene is:
The thick chloride that thick chloride basin is sent here initially enters de-heavy component tower, from obtaining D-D mixture at the bottom of this tower, through storage Tank reinstalls tank car as byproduct;
Obtain chloropropene and low boiling mixture, condensed device+complete condenser condensation from tower top, be then sent through rectifying column, at this tower Low-boiling-point substance is isolated at top;Described low-boiling-point substance condenses through recirculated water cooling condenser, sends into tank field low-boiling-point substance basin;Obtain at the bottom of tower >= The chloropropene product of 98%, sends into tank field chloropropene basin;
De-heavy component tower is atmospheric tower, and tower top uses recirculated water+chilled water B-grade condensation, and rectifying column is pressurizing tower, tower top Using recirculated water to condense under pressurised conditions, condensation efficiency is all not less than 99%;
The described coolant in condenser is recirculated water, and the described coolant in complete condenser is chilled brine.
Hydrogen chloride absorption become hydrochloric acid step particularly as follows:
Condensation steams the hydrogen chloride in the propylene of tower top and chlorine hydride mixed gas body and uses level Four absorption technique, described four Level absorption technique is: absorption by Hydrochloric Acid one tower+absorption by Hydrochloric Acid two towers+caustic wash tower+water scrubber;
Mixed gas initially enters absorption by Hydrochloric Acid one tower, absorbs through circulating cooling, obtains the hydrochloric acid of concentration >=30%, send Enter hydrochloric acid basin, after tinning, send battery limit (BL), as byproduct;
Being entered absorption by Hydrochloric Acid two tower by propylene containing a small amount of hydrogen chloride after absorbing, water cyclic absorption obtains watery hydrochloric acid, Sending hydrochloric acid absorption tower to use, this propylene enters back into caustic wash tower, washs with the NaOH solution circulation of 3~10%, in complete for hydrogen chloride And absorption, the propylene after alkali cleaning through washing, enters back into propylene compressor again;
The HCl gas that the hydrochloric acid trough of acid absorption column and dilute acid bath volatilize, enters tail gas absorber water absorption, absorbing liquid Entering dilute acid bath, unabsorbed a small amount of HCl gas empties through 16m aiutage;Collect alkali cleaning, the brine waste of washing generation.
Concretely comprising the following steps of propylene pressure recovery:
Propylene after depickling enters surge tank, separates a part of mechanical water, enters propylene compressor one section compression, outlet pressure Power reaches 0.35~0.4MPa, after compressor built-in oil eliminator oil removing, cooler refrigerated separation moisture, enters back into two sections of pressures Contracting, outlet pressure is 1.6MPa, after compressor built-in oil eliminator oil removing, cooler refrigerated separation moisture, through secondary cycle Water-cooled is congealed into propylene liguid, delivers to circulate propylene tank, enters back into subcooler after separated moisture, freezing through the propylene of dry propylene tank And entering molecular sieve drying system after separating moisture, dried propylene removes dry propylene tank, utilizes as feedstock circulation.
The beneficial effects of the present invention is, use the chloropropene that assembly of the invention prepares, its yield is from tradition side The 75-80% of method brings up to 80-85%, and it is less to use assembly of the invention to carry out reacting its side reaction, and production efficiency is high.
Accompanying drawing explanation
Fig. 1 is the chloropropene process units structural representation of the present invention;
In figure, 1-propylene tank, 2-dehydrator, 3-dry propylene tank, 4-propylene subcooler, 5-condenser, 6-chloride cools down Device, 7-steamer, 8-propylene surge tank, 9-heat exchanger, 10-chlorination reactor, 11-chlorine evaporimeter, 12-chlorine buffers Tank.
Detailed description of the invention
With detailed description of the invention, the present invention is further described below in conjunction with the accompanying drawings, in order to the technology of this area Personnel know more about the present invention, but do not limit the present invention with this.
The process units of chloropropene, this device includes following structure:
Propylene tank 1 is parallel with dehydrator 2 and dry propylene tank 1 by pipeline, and dry propylene tank 1 is in series with propylene subcooler 4, and third The other end of alkene subcooler 4 is parallel with condensation and steams tower and chloride cooler 6, condensation steam tower and chloride cooler 6 with Steamer 7 is in series, and the other end of steamer 7 has been sequentially connected in series propylene surge tank 8, heat exchanger 9 and chloride reactor;
The other end of chloride reactor has been sequentially connected in series chlorine evaporimeter 11 and Chlorine Buffer Vessel 12.
Liquid chlorine enters Chlorine Buffer Vessel 12 after chlorine evaporimeter 11 gasifies, by delivering to chlorination reactor 10 after metering Mixing section;
Whether the propylene tank 1 that raw material propylene is sent into tank field stores, need dehydration to enter back into dry third according to the moisture content of propylene Alkene tank 1;Then divide two-way with the Propylene recovery in dry propylene tank 1, described raw material propylene and Propylene recovery are at propylene subcooler 4 Mutually after heat exchange, a road flows to condensation and steams column overhead spray refrigeration, and another road is steamed entering condensation through perchlorhydria cooler 6 Go out the reaction mass cooling of tower, and make entrance steamer 7 after self vaporization, after completely vaporizing, enter propylene surge tank 8;
The described propylene after vaporization enters heat exchanger 9 after metering, by chlorination reactor 10 reactant out Propylene after expecting vaporization is preheated to 360 DEG C and enters chlorination reactor 10 mixing section, and propylene and chlorine are equal with the mol ratio of 4-6:1 Enter reactor after even mixing and carry out high-temperature chlorination;
Reaction product include chloropropene, 1,2-dichloropropane+1,3-dichloropropylene, the propylene of excess, hydrogen chloride mixed Close gas;
The thick chloropropene of reaction product material and hydrogen chloride pass through and propylene heat exchange, and reaction propylene is preheated to uniform temperature, Reaction mass steams the propylene heat exchange of column overhead again with condensation, then cools down to chloride cooler 6 through liquid reactions propylene, cold But enter condensation to about-10 DEG C and steam tower;
Thick chloropropene and HCl separation in condensation steams tower, hydrogen chloride becomes hydrochloric acid through absorption, and propylene is through overvoltage It is recycled to propylene tank 1 after contracting, recycles;
Thick chloride squeezes into tank field semi-finished product tank through pump, in rectifying column rectifying and purification, obtains finished product chloropropene;
Described reaction equation is:
CH3-CH=CH2+Cl2 CH2Cl-CH=CH2 + HCl
CH3-CH=CH2+Cl2 CH3-CHCl-CH2Cl
CH2Cl-CH=CH2+Cl2 CH2Cl-CH=CHCl+HCl
CH3-CH2-CH3+Cl2 CH3-CH2-CH2Cl+HCl
CH3CH=CH2+3Cl2 3C+6HCl。
Propylene is 5:1 with the mol ratio of chlorine.
When its moisture content of raw material propylene is less than or equal to 10ppm, propylene is directly entered dry propylene tank 3;
When its moisture content of raw material propylene is more than 10ppm, by raw material propylene dehydration to its moisture content less than or equal to 10ppm Rear feeding dry propylene tank 3.
Above-mentioned thick chloride refines the step for finished product chloropropene:
The thick chloride that thick chloride basin is sent here initially enters de-heavy component tower, from obtaining D-D mixture at the bottom of this tower, through storage Tank reinstalls tank car as byproduct;
Obtaining chloropropene and low boiling mixture from tower top, condensed device 5+ complete condenser condenses, and is then sent through rectifying column, at this tower Low-boiling-point substance is isolated at top;Described low-boiling-point substance condenses through recirculated water cooling condenser 5, sends into tank field low-boiling-point substance basin;Obtain at the bottom of tower The chloropropene product of >=98%, sends into tank field chloropropene basin;
De-heavy component tower is atmospheric tower, and tower top uses recirculated water+chilled water B-grade condensation, and rectifying column is pressurizing tower, tower top Using recirculated water to condense under pressurised conditions, condensation efficiency is all not less than 99%;
The described coolant in condenser 5 is recirculated water, and the described coolant in complete condenser is chilled brine.
Above-mentioned hydrogen chloride absorption become hydrochloric acid step particularly as follows:
Condensation steams the hydrogen chloride in the propylene of tower top and chlorine hydride mixed gas body and uses level Four absorption technique, described four Level absorption technique is: absorption by Hydrochloric Acid one tower+absorption by Hydrochloric Acid two towers+caustic wash tower+water scrubber;
Mixed gas initially enters absorption by Hydrochloric Acid one tower, absorbs through circulating cooling, obtains the hydrochloric acid of concentration >=30%, send Enter hydrochloric acid basin, after tinning, send battery limit (BL), as byproduct;
Being entered absorption by Hydrochloric Acid two tower by propylene containing a small amount of hydrogen chloride after absorbing, water cyclic absorption obtains watery hydrochloric acid, Sending hydrochloric acid absorption tower to use, this propylene enters back into caustic wash tower, washs with the NaOH solution circulation of 3~10%, in complete for hydrogen chloride And absorption, the propylene after alkali cleaning through washing, enters back into propylene compressor again;
The HCl gas that the hydrochloric acid trough of acid absorption column and dilute acid bath volatilize, enters tail gas absorber water absorption, absorbing liquid Entering dilute acid bath, unabsorbed a small amount of HCl gas empties through 16m aiutage;Collect alkali cleaning, the brine waste of washing generation.
Concretely comprising the following steps of above-mentioned propylene pressure recovery:
Propylene after depickling enters surge tank, separates a part of mechanical water, enters propylene compressor one section compression, outlet pressure Power reaches 0.35~0.4MPa, after compressor built-in oil eliminator oil removing, cooler refrigerated separation moisture, enters back into two sections of pressures Contracting, outlet pressure is 1.6MPa, after compressor built-in oil eliminator oil removing, cooler refrigerated separation moisture, through secondary cycle Water-cooled is congealed into propylene liguid, delivers to circulate propylene tank 1, enters back into subcooler after separated moisture, cold through the propylene of dry propylene tank Entering molecular sieve drying system after freezing and separating moisture, dried propylene removes dry propylene tank, utilizes as feedstock circulation.
According to the characteristic of molecular sieve, its individuality having a certain size aperture, energy binding molecule diameter is less than the water in aperture Molecule, is not adsorbed more than the propylene in aperture, and temperature is the lowest, and adsorption effect is the best, can adsorb substantial amounts of water at normal temperatures. Along with increase and the continuous expansion of adsorbance of the time of use, dehydrating effect is gradually deteriorated, and at this moment progressivelyes reach " breakthrough point ", just Needing to regenerate molecular sieve, be accomplished by changing molecular sieve when regeneration effect is bad, molecular sieve is changed once for 2 years.
Molecular sieve drying system is with two adsorption dehumifier parallel connections, and a job, another can be dewatered again simultaneously Raw process, alternates work and regeneration, and to ensure that equipment runs continuously, drier works at 5 DEG C.Regenerating molecular sieve is profit With the pre-hot nitrogen of steam heater and electric heater to 200 DEG C of undershoot nitrogen regenerations, hot nitrogen is utilized to make point to molecular sieve heating Moisture in son sieve becomes steam, and nitrogen is taken out of in drier after a small amount of propylene of moisture and residual, (follows through carrier gas water cooler Ring water-cooled is coagulated) and the condensation of chilled water cooler, moisture separates after substantially completely condensing.Regeneration in general one week once, continues every time Time 8h, nitrogen usage amount 50m3/ time.After regeneration, in molecular sieve drying system, the nitrogen containing propylene is through charcoal absorption 48m aiutage discharge after process.

Claims (1)

1. the process units of chloropropene, it is characterised in that described device includes following structure:
Propylene tank is parallel with dehydrator and dry propylene tank by pipeline, and dry propylene tank is in series with propylene subcooler, propylene subcooler The other end be parallel with condensation and steam tower and chloride cooler, condensation steams tower and goes here and there mutually with steamer with chloride cooler Connection, the other end of steamer has been sequentially connected in series propylene surge tank, heat exchanger and chloride reactor;
The other end of chloride reactor has been sequentially connected in series chlorine evaporimeter and Chlorine Buffer Vessel;
Liquid chlorine enters Chlorine Buffer Vessel after chlorine evaporimeter gasifies, by delivering to the mixing section of chlorination reactor after metering;
Whether the propylene tank that raw material propylene is sent into tank field stores, need dehydration to enter back into dry propylene tank according to the moisture content of propylene; Then divide two-way with the Propylene recovery in dry propylene tank, described raw material propylene and Propylene recovery are in the mutual heat exchange of propylene subcooler After, a road flows to condensation and steams column overhead spray refrigeration, and another road steams the anti-of tower through perchlorhydria cooler to entering condensation Answer material to cool down, and make entrance steamer after self vaporization, after completely vaporizing, enter propylene surge tank;
The described propylene after vaporization enters heat exchanger after metering, will vaporization by chlorination reactor reaction mass out After propylene be preheated to 360 DEG C enter chlorination reactor mixing sections, propylene uniformly mixes laggard with chlorine with the mol ratio of 4-6:1 Enter reactor and carry out high-temperature chlorination;
Reaction product includes chloropropene, 1,2-dichloropropane+1,3-dichloropropylene, the propylene of excess, the gaseous mixture of hydrogen chloride Body;
The thick chloropropene of reaction product material and hydrogen chloride pass through and propylene heat exchange, and reaction propylene is preheated to uniform temperature, reaction Material steams the propylene heat exchange of column overhead again with condensation, then cools down to chloride cooler through liquid reactions propylene, be cooled to- About 10 DEG C enter condensation and steam tower;
Thick chloropropene and HCl separation in condensation steams tower, hydrogen chloride becomes hydrochloric acid through absorption, and propylene is after overcompression It is recycled to propylene tank, recycles;
Thick chloride squeezes into tank field semi-finished product tank through pump, in rectifying column rectifying and purification, obtains finished product chloropropene;
Described reaction equation is:
CH3-CH=CH2+Cl2 CH2Cl-CH=CH2 + HCl
CH3-CH=CH2+Cl2 CH3-CHCl-CH2Cl
CH2Cl-CH=CH2+Cl2 CH2Cl-CH=CHCl+HCl
CH3-CH2-CH3+Cl2 CH3-CH2-CH2Cl+HCl
CH3CH=CH2+3Cl2 3C+6HCl;
Propylene is 5:1 with the mol ratio of chlorine;
When its moisture content of raw material propylene is less than or equal to 10ppm, propylene is directly entered dry propylene tank;
When its moisture content of raw material propylene is more than 10ppm, raw material propylene dehydration is sent to its moisture content less than or equal to after 10ppm Enter dry propylene tank;
Above-mentioned thick chloride refines the step for finished product chloropropene:
The thick chloride that thick chloride basin is sent here initially enters de-heavy component tower, from obtaining D-D mixture at the bottom of this tower, through basin again Load tank car as byproduct;
Obtain chloropropene and low boiling mixture, condensed device+complete condenser condensation from tower top, be then sent through rectifying column, at this top of tower Isolate low-boiling-point substance;Described low-boiling-point substance condenses through recirculated water cooling condenser, sends into tank field low-boiling-point substance basin;>=98% is obtained at the bottom of tower Chloropropene product, send into tank field chloropropene basin;
De-heavy component tower is atmospheric tower, and tower top uses recirculated water+chilled water B-grade condensation, and rectifying column is pressurizing tower, and tower top uses Recirculated water condenses under pressurised conditions, and condensation efficiency is all not less than 99%;
The described coolant in condenser is recirculated water, and the described coolant in complete condenser is chilled brine;
Above-mentioned hydrogen chloride absorption become hydrochloric acid step particularly as follows:
Condensation steams the hydrogen chloride in the propylene of tower top and chlorine hydride mixed gas body and uses level Four absorption technique, described level Four to inhale Skill of knocking off is: absorption by Hydrochloric Acid one tower+absorption by Hydrochloric Acid two towers+caustic wash tower+water scrubber;
Mixed gas initially enters absorption by Hydrochloric Acid one tower, absorbs through circulating cooling, obtains the hydrochloric acid of concentration >=30%, sends into salt Acid basin, sends battery limit (BL), as byproduct after tinning;
Being entered absorption by Hydrochloric Acid two tower by propylene containing a small amount of hydrogen chloride after absorbing, water cyclic absorption obtains watery hydrochloric acid, send salt Acid absorption column uses, and this propylene enters back into caustic wash tower, washs with the NaOH solution circulation of 3~10%, hydrogen chloride neutralizes suction completely Receiving, the propylene after alkali cleaning through washing, enters back into propylene compressor again;
The HCl gas that the hydrochloric acid trough of acid absorption column and dilute acid bath volatilize, enters tail gas absorber water absorption, and absorbing liquid enters Dilute acid bath, unabsorbed a small amount of HCl gas empties through 16m aiutage;Collect alkali cleaning, the brine waste of washing generation;
Concretely comprising the following steps of above-mentioned propylene pressure recovery:
Propylene after depickling enters surge tank, separates a part of mechanical water, enters propylene compressor one section compression, and outlet pressure reaches 0.35~0.4MPa, after compressor built-in oil eliminator oil removing, cooler refrigerated separation moisture, enter back into two sections of compressions, go out Mouth pressure is 1.6MPa, after compressor built-in oil eliminator oil removing, cooler refrigerated separation moisture, coagulates through secondary cycle water-cooled Become propylene liguid, deliver to circulate propylene tank, after separated moisture, enter back into subcooler, freezing through the propylene of dry propylene tank and separate Entering molecular sieve drying system after moisture, dried propylene removes dry propylene tank, utilizes as feedstock circulation;
Molecular sieve drying system is with two adsorption dehumifier parallel connections, and a job, another carries out dehydration regeneration process, phase simultaneously Alternation and regeneration mutually, drier works at 5 DEG C one week and regenerates once, each duration 8h, nitrogen usage amount 50m3/ Secondary, after regeneration, in molecular sieve drying system, the nitrogen 48m aiutage after charcoal absorption processes containing propylene discharges.
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CN104860789A (en) * 2015-05-21 2015-08-26 山东海益化工科技有限公司 Method for recovering propylene in preparation process of chloropropene
CN104876793A (en) * 2015-05-21 2015-09-02 山东海益化工科技有限公司 Chloropropene refining process
CN104876792A (en) * 2015-05-21 2015-09-02 山东海益化工科技有限公司 Method for producing high-purity chloropropene
CN105037075A (en) * 2015-05-21 2015-11-11 山东海益化工科技有限公司 Processing technology of hydrogen chloride in propylene preparation process
CN104892354A (en) * 2015-05-21 2015-09-09 山东海益化工科技有限公司 Chlorination method and chlorination device in chloropropene production process
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