CN108456131A - The vapo r recompression formula manufacturing device and manufacturing method of dichlorohydrin - Google Patents
The vapo r recompression formula manufacturing device and manufacturing method of dichlorohydrin Download PDFInfo
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- CN108456131A CN108456131A CN201710086228.0A CN201710086228A CN108456131A CN 108456131 A CN108456131 A CN 108456131A CN 201710086228 A CN201710086228 A CN 201710086228A CN 108456131 A CN108456131 A CN 108456131A
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- destilling tower
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- DEWLEGDTCGBNGU-UHFFFAOYSA-N 1,3-dichloropropan-2-ol Chemical compound ClCC(O)CCl DEWLEGDTCGBNGU-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 128
- 230000006835 compression Effects 0.000 claims abstract description 55
- 238000007906 compression Methods 0.000 claims abstract description 55
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 24
- 239000007864 aqueous solution Substances 0.000 claims abstract description 22
- 235000011187 glycerol Nutrition 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims description 67
- 239000012071 phase Substances 0.000 claims description 40
- 239000012074 organic phase Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000004821 distillation Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 description 182
- 239000007789 gas Substances 0.000 description 118
- -1 chloropropyl alcohol Chemical compound 0.000 description 17
- 238000010586 diagram Methods 0.000 description 10
- 238000009833 condensation Methods 0.000 description 8
- 230000005494 condensation Effects 0.000 description 8
- 238000005265 energy consumption Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- 238000010025 steaming Methods 0.000 description 6
- 125000003963 dichloro group Chemical group Cl* 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 5
- 238000005192 partition Methods 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 208000012839 conversion disease Diseases 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- OWXJKYNZGFSVRC-NSCUHMNNSA-N (e)-1-chloroprop-1-ene Chemical compound C\C=C\Cl OWXJKYNZGFSVRC-NSCUHMNNSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- XEPXTKKIWBPAEG-UHFFFAOYSA-N 1,1-dichloropropan-1-ol Chemical compound CCC(O)(Cl)Cl XEPXTKKIWBPAEG-UHFFFAOYSA-N 0.000 description 1
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000003225 biodiesel Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- NJTGANWAUPEOAX-UHFFFAOYSA-N molport-023-220-454 Chemical compound OCC(O)CO.OCC(O)CO NJTGANWAUPEOAX-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- WHFQAROQMWLMEY-UHFFFAOYSA-N propylene dimer Chemical compound CC=C.CC=C WHFQAROQMWLMEY-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/62—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by introduction of halogen; by substitution of halogen atoms by other halogen atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of manufacturing device and manufacturing method of dichlorohydrin, and dichlorohydrin is generated suitable for making glycerine be reacted in the environment of there are catalyst with hydrochloride aqueous solution.The manufacturing device of dichlorohydrin includes an at least reactor, the first destilling tower, the first phase-splitter, first gas compression set and the first heat-exchange device.First destilling tower is connected to an at least reactor.First phase-splitter is connected to the tower top of the first destilling tower with first gas compression set.First heat-exchange device is connected to via first flow path between first gas compression set and the first phase-splitter, and the side wall of the first destilling tower is connected to via second flow path.The manufacturing device and manufacturing method of the dichlorohydrin can reduce the manufacturing cost of dichlorohydrin.
Description
Technical field
The present invention relates to a kind of manufacturing method of dichlorohydrin more particularly to a kind of steamings of the dichlorohydrin with phase-splitter
Gas recompresses formula manufacturing device and manufacturing method.
Background technology
The main preparation methods of dichlorohydrin (dichloropropanol) are propylene (propene) high-temp chlorination at present
Method, it includes two steps：Make acrylonitrile-chlorinated generation chloropropene (allyl chloride) at high temperature, and uses excessive work
Industry water makes chloropropene form dichlorohydrin with chlorination reaction.However, will produce a large amount of waste water using propylene high-temperature chloridising
With other waste materials, therefore cause technology and environmentally the problem of.
Therefore, it develops and a kind of with chlorinating agent directly reacting generation in the case of catalyst using glycerine (glycerol)
The method of dichlorohydrin, the method not will produce a large amount of waste water and waste material, therefore be a kind of more economical and environmentally friendly manufacturing method.
However, when preparing dichlorohydrin using the method, the azeotropic mixture (azeotrope) of dichlorohydrin and water can be formed,
If extractant (extractant) is added obtains dichlorohydrin with separating azeotrope, manufacturing cost, and extractant will be improved
Azeotropic mixture may be formed with catalyst and cause difficulty of the catalyst on recycling.
Invention content
The present invention provides a kind of manufacturing device and manufacturing method of dichlorohydrin, can reduce the manufacturing cost of dichlorohydrin.
The present invention provides a kind of manufacturing device of dichlorohydrin, suitable for making glycerine there is catalysis with hydrochloride aqueous solution
It is reacted in the environment of agent and generates dichlorohydrin.The manufacturing device of dichlorohydrin includes an at least reactor, the first distillation
Tower, the first phase-splitter, first gas compression set and the first heat-exchange device.First destilling tower is connected at least one reaction
Device.First phase-splitter is connected to the tower top of the first destilling tower.First gas compression set is connected to the tower top of the first destilling tower.The
One heat-exchange device is connected to via first flow path between first gas compression set and the first phase-splitter, and via second flow path
It is connected to the side wall of the first destilling tower.
In one embodiment of this invention, the manufacturing device of above-mentioned dichlorohydrin further includes the first waterworks, directly
It is connected to the first phase-splitter.
In one embodiment of this invention, the gas from first gas compression set in first flow path with the
After the liquid being derived from the first destilling tower in two flow paths carries out heat exchange in the first heat-exchange device, it flow to first respectively
Phase-splitter and the first destilling tower.
In one embodiment of this invention, the manufacturing device of above-mentioned dichlorohydrin further include second gas compression set with
Second heat-exchange device.First gas compression set is connected between the tower top of the first destilling tower and second gas compression set.
Second heat-exchange device is connected to via third flow path between second gas compression set and the first phase-splitter, and via the 4th stream
Road is connected to side wall or the bottom of tower of the first destilling tower.
In one embodiment of this invention, the gas from second gas compression set in third flow path with the
After the liquid in the first destilling tower in four flow paths carries out heat exchange in the second heat-exchange device, it flow to the first phase-splitter respectively
With the first destilling tower.
In one embodiment of this invention, the manufacturing device of above-mentioned dichlorohydrin further includes after-fractionating tower.First steams
Tower is evaporated to be connected at least between a reactor and after-fractionating tower.
In one embodiment of this invention, the manufacturing device of above-mentioned dichlorohydrin further includes heat exchange pipe, is connected to
Between the bottom of tower of first destilling tower and the feed inlet of after-fractionating tower, so that the liquid of the bottom of tower of the first destilling tower is along heat exchange
Pipeline flow to the feed inlet of after-fractionating tower, and the portion gas in after-fractionating tower is made to be back to first along heat exchange pipe
The bottom of tower of destilling tower.
In one embodiment of this invention, the first above-mentioned destilling tower includes partition wall, by the internal stretch of the first destilling tower
To top, the top of the first destilling tower is divided into first chamber and second chamber.
In one embodiment of this invention, above-mentioned first gas compression set is connected to the top of first chamber, and
One heat-exchange device is connected to the side wall of first chamber via second flow path.
In one embodiment of this invention, the manufacturing device of above-mentioned dichlorohydrin further includes the second phase-splitter, third gas
Body compression set and third heat-exchange device.Second phase-splitter is connected to the top of second chamber with third gas compression set
Portion.Third heat-exchange device is connected to via the 5th flow path between third gas compression set and the second phase-splitter, and via
Six flow paths are connected to the side wall of second chamber.
In one embodiment of this invention, the gas of third gas compression set is derived from the 5th flow path and the 6th
After the liquid being derived from second chamber in flow path carries out heat exchange in third heat-exchange device, it flow to the second phase-splitter respectively
With second chamber.
In one embodiment of this invention, the first above-mentioned destilling tower is exported including the first effluent, to take out the first effluent
Product.First side draw product includes the water of purity 85% to 100%.
One embodiment of the invention provides a kind of manufacturing method of dichlorohydrin, suitable for making glycerine and hydrochloride aqueous solution
It is reacted in the environment of there are catalyst and generates dichlorohydrin.The manufacturing method of dichlorohydrin includes the following steps.
In an at least reactor, glycerine is made to be reacted in the environment of there are catalyst with hydrochloride aqueous solution, and generates initial production
Object.So that the from initial product first charging is entered the first destilling tower for being connected with the first phase-splitter, and generates the first tower top
Product and the first tower bottom product.So that the first overhead product of part is entered first gas compression set and generates the first compression production
Object.So that the first compressed product is passed through first flow path and flow to the first phase-splitter through the first heat-exchange device, in the first phase-splitter
It forms the first water-phase product and includes the first organic phase product of dichlorohydrin.Keep the liquid that the side wall of the first destilling tower flows out logical
It crosses second flow path and is back to the first destilling tower, the first compressed product and second wherein in first flow path through the first heat-exchange device
Liquid in flow path carries out heat exchange in the first heat-exchange device.Take out the first organic phase product.
In one embodiment of this invention, the manufacturing method of above-mentioned dichlorohydrin further includes that the first waterworks are direct
It is connected to the first phase-splitter.
In one embodiment of this invention, the manufacturing method of above-mentioned dichlorohydrin further includes that the first tower top of part is made to produce
Object enters first phase-splitter, wherein the first overhead product and the first compressed product in the first phase-splitter form the first water
Phase product and the first organic phase product.
In one embodiment of this invention, the manufacturing method of above-mentioned dichlorohydrin further includes making the first of part to compress production
Object enters second gas compression set and generates the second compressed product.Make the second compressed product pass through third flow path to hand over through the second heat
Changing device flow to the first phase-splitter, wherein the first compressed product in the first phase-splitter forms the first water with the second compressed product
Phase product and the first organic phase product.The liquid of the side wall or bottom of tower outflow that make the first destilling tower passes through the 4th flow path through the second heat
Switch is back to the first destilling tower.The second compressed product in third flow path is handed over the liquid in the 4th flow path in the second heat
Heat exchange is carried out in changing device.
In one embodiment of this invention, the manufacturing method of above-mentioned dichlorohydrin further includes making the bottom of tower of the first destilling tower
Liquid enter after-fractionating tower along heat exchange pipe, and generate the second overhead product and the second tower bottom product.After-fractionating
Portion gas in tower is back to the bottom of tower of the first destilling tower along heat exchange pipe.
In one embodiment of this invention, the first above-mentioned destilling tower includes partition wall, by the internal stretch of the first destilling tower
To top, the top of the first destilling tower is divided into first chamber and second chamber.
In one embodiment of this invention, the first above-mentioned overhead product enters the first phase-splitter from first chamber, and certainly
The liquid of the side wall outflow of first chamber is back to first chamber by second flow path through the first heat-exchange device.
In one embodiment of this invention, the manufacturing method of above-mentioned dichlorohydrin further includes that the first tower top of part is made to produce
Object enters third gas compression set from second chamber and generates third compressed product.Third compressed product is set to pass through the 5th flow path
Flow to the second phase-splitter through third heat-exchange device, and formed in the second phase-splitter the second water-phase product with include dichlorohydrin
Second Organic Phase product.Make the liquid flowed out from the side wall of second chamber pass through the 6th flow path to flow back through third heat-exchange device
To second chamber, wherein third compressed product in the 5th flow path and the liquid in the 6th flow path in third heat-exchange device into
Row heat exchange.Take out Second Organic Phase product.
In one embodiment of this invention, the manufacturing method of above-mentioned dichlorohydrin further includes that the first tower top of part is made to produce
Object enters the second phase-splitter from second chamber, wherein the first overhead product in the second phase-splitter is formed with third compressed product
Second water-phase product and Second Organic Phase product.
In one embodiment of this invention, the manufacturing method of above-mentioned dichlorohydrin further includes the tower top in the first destilling tower
Take out the first side draw product in the first effluent exit between bottom of tower.First side draw product include purity be 85wt% extremely
The water of 100wt%.
Based on above-mentioned, dichlorohydrin is taken out using phase-splitter separating azeotrope, can avoid additional addition extractant, therefore can
Reduce the manufacturing cost of dichlorohydrin.Furthermore it can avoid extractant to form azeotropic mixture with catalyst and catalyst is caused to be difficult to follow
The problem of ring utilizes.In addition, can be with destilling tower in heat-exchange device through the compressed high temperature and high pressure gas of gas compressing apparatus
Liquid carry out heat exchange, carry out detaching required partial heat energy to provide destilling tower, and then the energy needed for destilling tower can be reduced
Consumption.Therefore, the manufacturing cost of dichlorohydrin can further be reduced.
To make the foregoing features and advantages of the present invention clearer and more comprehensible, special embodiment below, and coordinate shown attached drawing
It is described in detail below.
Description of the drawings
Figure 1A and Figure 1B are respectively the schematic diagram of the manufacturing device of the dichlorohydrin of an embodiment and two according to the present invention
The manufacturing flow chart of chloropropyl alcohol.
Fig. 2A and Fig. 2 B are respectively the schematic diagram of the manufacturing device of the dichlorohydrin of an embodiment and two according to the present invention
The manufacturing flow chart of chloropropyl alcohol.
Fig. 3 A and Fig. 3 B are respectively the schematic diagram of the manufacturing device of the dichlorohydrin of an embodiment and two according to the present invention
The manufacturing flow chart of chloropropyl alcohol.
Fig. 4 A and Fig. 4 B are respectively the schematic diagram of the manufacturing device of the dichlorohydrin of an embodiment and two according to the present invention
The manufacturing flow chart of chloropropyl alcohol.
Fig. 5 A and Fig. 5 B are respectively the schematic diagram of the manufacturing device of the dichlorohydrin of an embodiment and two according to the present invention
The manufacturing flow chart of chloropropyl alcohol.
Specific implementation mode
Figure 1A and Figure 1B are respectively the schematic diagram of the manufacturing device of the dichlorohydrin of an embodiment and two according to the present invention
The manufacturing flow chart of chloropropyl alcohol.
Figure 1A is please referred to, the present embodiment provides a kind of manufacturing devices 100 of dichlorohydrin, suitable for making glycerine and hydrogen chloride
Aqueous solution is reacted in the environment of there are catalyst and generates dichlorohydrin.The manufacturing device 100 of dichlorohydrin includes extremely
A few reactor 102, destilling tower 108, phase-splitter 110, gas compressing apparatus 116 and heat-exchange device 118.Destilling tower 108
It is connected to reactor 102.Phase-splitter 110 is connected to the tower top of destilling tower 108 with gas compressing apparatus 116.Heat-exchange device 118
It is connected between gas compressing apparatus 116 and phase-splitter 110 via flow path P1, and destilling tower 108 is connected to via flow path P2
Side wall.
In one embodiment, the manufacturing device 100 of dichlorohydrin may also include waterworks 120, be connected directly to point
Phase device 110.The gas from gas compressing apparatus 116 in flow path P1 is derived from destilling tower 108 in flow path P2
In liquid heat exchange can be carried out in heat-exchange device 118, and then flow to phase-splitter 110 and destilling tower 108 respectively.Separately
Outside, destilling tower 108 may also include effluent outlet S1, to take out side draw product.The side draw product of destilling tower 108 may include purity
85% to 100% water.In other embodiments, the purity of the water in the side draw product of destilling tower 108 can be for 90wt% extremely
99.99wt%, most preferably 95wt% are to 99.95wt%.
Referring to Figure 1A and Figure 1B, the present embodiment also provides a kind of manufacturing method of dichlorohydrin, including following step
Suddenly.First, step S100 is carried out, in an at least reactor 102, makes glycerine and hydrochloride aqueous solution there are the rings of catalyst
It is reacted under border, and generates initial product.Reactor 102 may include flow reactor or batch reactor.In this implementation
It is to be illustrated by taking a reactor 102 as an example, but the present invention is not limited thereto, in this technical field technology people in example
Member can adjust the quantity of reactor 102 according to process design.In one embodiment, the pair of production biodiesel can be used in glycerine
Product or chemically synthesized glycerine.Catalyst may include acetic acid or adipic acid.Initial product includes dichlorohydrin and a chloropropyl alcohol,
Wherein dichlorohydrin is principal product, and a chloropropyl alcohol is intermediate product.It is water-soluble that initial product may also include unreacted hydrogen chloride
Liquid, glycerine and catalyst.
Then, step S102 is optionally carried out, initial product is made to enter destilling tower 104 as charging, and generates tower
Push up product and tower bottom product.Initial product can be reacted and be detached in destilling tower 104.In one embodiment, destilling tower 104
There can be reboiler (reboiler) 106, carry out detaching required thermal energy to provide destilling tower 104.The bottom of tower of destilling tower 104
Product mainly include unreacted glycerine, may also include a small amount of dichlorohydrin, an a small amount of chloropropyl alcohol, a small amount of hydrochloride aqueous solution with
Catalyst.The tower bottom product of destilling tower 104 is reflowable to continuing to recycle in reactor 102, to increase reaction conversion ratio.It steams
The overhead product for evaporating tower 104 include a large amount of dichlorohydrins, a large amount of chloropropyl alcohols, a large amount of hydrochloride aqueous solutions, catalyst with it is a small amount of
Glycerine.
Step S104 is carried out, the charging from initial product is made to enter the destilling tower 108 for being connected with phase-splitter 110, and
Generate overhead product and tower bottom product.In the present embodiment, the overhead product of destilling tower 104 can be used as the charging of destilling tower 108,
And it is reacted and is detached in destilling tower 108.Specifically, the overhead product of destilling tower 104 can be condensed via condenser 105
It is stored in afterwards in backflash 107, can then be partly refluxed to destilling tower 104 and part flow to destilling tower 108.Destilling tower 108
There can be reboiler 112, carry out detaching required thermal energy to provide destilling tower 108.A large amount of dichlorohydrin in destilling tower 108
The lower azeotropic mixture of boiling point can be formed with water, and form the overhead product of destilling tower 108, therefore the overhead product of destilling tower 108
In dichlorohydrin content can be more than destilling tower 108 tower bottom product in dichlorohydrin content.The tower top of destilling tower 108
Product may also include a chloropropyl alcohol and hydrochloride aqueous solution.The tower bottom product of destilling tower 108 include a large amount of hydrochloride aqueous solutions with
A large amount of catalyst, and may also include a small amount of dichlorohydrin and a small amount of glycerine.In addition, the manufacturer of the dichlorohydrin in the present embodiment
Further include the effluent outlet places the S1 taking-up side draw product between the tower top and bottom of tower of destilling tower 108 comprising purity is in method
The water of 85wt% to 100wt%, the purity of water can be 90wt% to 99.99wt%, most preferably 95wt% in other embodiments
To 99.95wt%.From effluent outlet, S1 takes out the water (reaction product) of the high-purity of destilling tower 108, and the chemistry of reaction can be made flat
Weighing apparatus is carried out towards the direction for increasing reaction product, therefore the reaction conversion ratio and dichlorohydrin and/or a chlorine third of reactant can be improved
The yield of alcohol.
It in other embodiments, also can be without step S102.Thus, which the charging of destilling tower 108 can be reactor
102 initial product.In other words, the initial product of reactor 102 can enter directly into destilling tower 108.
Later, step S108, step S110a and step S110b can be carried out.Specifically, step S108 can be carried out first, make
The overhead product of the part of destilling tower 108 enters gas compressing apparatus 116 and generates compressed product.Gas compressing apparatus 116 can
The overhead product of the destilling tower 108 of compressed gaseous, to improve its temperature and pressure.Therefore, the compression production of gas compressing apparatus 116
The temperature of object can be higher than the temperature and pressure of the overhead product of destilling tower 108 with pressure.
Then, step S110a can be carried out, so that the compressed product of gas compressing apparatus 116 is passed through flow path P1 and is filled through heat exchange
It sets 118 and flow to phase-splitter 110.It is produced with the organic phase including dichlorohydrin thus, form water-phase product in phase-splitter 110
Object.While carrying out step S110a, step S110b can be carried out, the liquid that the side wall of destilling tower 108 flows out is made to pass through flow path P2
It is back to destilling tower 108 through heat-exchange device 118.The compressed product of gas compressing apparatus 116 in flow path P1 and flow path P2
In liquid heat exchange is carried out in heat-exchange device 118.Thus, which the temperature of the liquid flowed out from destilling tower 108 can be improved
Degree, so that it can heat destilling tower 108 when being back to destilling tower 108 along flow path P2.Therefore, the energy of reboiler 112 can be reduced
Consumption.On the other hand, the temperature of the compressed product of gas compressing apparatus 116 can be reduced, and it is made then to flow to phase-splitter 110.
It, can if total condensation is not low temperature liquid after the compressed product progress heat exchange of gas compressing apparatus 116 in one embodiment
Phase-splitter 110 is entered back into after so that it is condensed along the condensed devices 114 of flow path P1.In other embodiments, if gas compressing apparatus
116 compressed product carry out after heat exchange can total condensation be low temperature liquid, then can be flowed directly to without condenser 114 point
Phase device 110.
It is worth noting that, when the latent heat of the overhead product of destilling tower 108 is big and the tower top of destilling tower 108 and the temperature of bottom of tower
Difference is small, can save the energy consumption of more reboilers 112.In one embodiment, the overhead product of destilling tower 108 may include weight hundred
Divide the water than being greater than or equal to 80, at this time the compressed product (overhead product for being derived from destilling tower 108) of gas compressing apparatus 116
It can release a large amount of latent heat.In addition, the tower top of destilling tower 108 and the temperature difference of bottom of tower may be less than or equal to 25 DEG C.Thus, can
The whole energy consumption of destilling tower 108 is further decreased, namely further decreases the manufacturing cost of dichlorohydrin.
While carrying out step S108, step S110a and step S110b, step S106 can be carried out, destilling tower 108 is made
The overhead product of part enter phase-splitter 110.Thus, the overhead product and gas of the destilling tower 108 in phase-splitter 110
The compressed product of body compression set 116 forms the water-phase product and organic phase product of phase-splitter 110.It in one embodiment, can be
Condenser 114 is set between the tower top and phase-splitter 110 of destilling tower 108, so that the overhead product of the part of destilling tower 108 passes through
Condenser 114 enters back into phase-splitter 110 after condensing.
Organic phase product in phase-splitter 110 includes dichlorohydrin, and may also include a chloropropyl alcohol.The water of phase-splitter 110
Phase product includes hydrochloride aqueous solution, and water-phase product is reflowable to destilling tower 108.Since the density of water-phase product is less than organic
The density of phase product, therefore water-phase product is located at the upper layer of organic phase product.Phase-splitter 110 separates the azeotropic in destilling tower 108
Object and take out dichlorohydrin, therefore be not required to additionally add extractant.It is likely to form with catalyst thus, can avoid extractant
Azeotropic mixture and the problem of cause catalyst to be difficult to recycle.In one embodiment, waterworks 120 can be directly connected to point
Phase device 110.Waterworks 120 can directly adjust the hydrochloride aqueous solution concentration in phase-splitter 110, and can be by destilling tower 108
The compressed product of overhead product and gas compressing apparatus 116 effectively split-phase.
Then step S112 is carried out, the organic phase product in phase-splitter 110 is taken out, and obtains principal product dichlorohydrin.
In one embodiment, also the tower bottom product of destilling tower 108 can be made to be back in reactor 102, to recycle.
Based on above-described embodiment it is found that taking out dichlorohydrin by using 110 separating azeotrope of phase-splitter, volume can avoid
Outer addition extractant and manufacturing cost can be reduced.Furthermore it can avoid extractant to be likely to form azeotropic mixture with catalyst and cause to urge
Agent is difficult to the problem of recycling.In addition, make the compressed product of gas compressing apparatus 116 in heat-exchange device 118 with steaming
The liquid evaporated in tower 108 carries out heat exchange, it is possible to provide destilling tower 108 carries out detaching required partial heat energy, and then can reduce steaming
Evaporate the energy consumption needed for tower 108.Therefore, the manufacturing cost of dichlorohydrin can further be reduced.
Fig. 2A and Fig. 2 B are respectively the schematic diagram of the manufacturing device of the dichlorohydrin of an embodiment and two according to the present invention
The manufacturing flow chart of chloropropyl alcohol.
Please refer to Fig. 2A, the manufacture of the manufacturing device 200 and dichlorohydrin shown in figure 1A of the dichlorohydrin of the present embodiment
Device 100 is similar, and the manufacturing device 200 of dichlorohydrin may also include gas compressing apparatus 202 and heat-exchange device 204.Gas
Body compression set 116 is connected between the tower top of destilling tower 108 and gas compressing apparatus 202.Heat-exchange device 204 is via flow path
P3 is connected between gas compressing apparatus 202 and phase-splitter 110, and is connected to destilling tower 108 via flow path P4.In the present embodiment
In, heat-exchange device 204 can be connected to the side wall of destilling tower 108 via flow path P4.In other embodiments, heat-exchange device
204 can also be connected to the bottom of tower of destilling tower 108 via flow path P4.The gas from gas compressing apparatus 202 in flow path P3
Body can carry out heat exchange with the liquid from destilling tower 108 in flow path P4 in heat-exchange device 204, and can then divide
It does not flow to phase-splitter 110 and destilling tower 108.
Referring to Fig. 2A and Fig. 2 B, the manufacturing method of the dichlorohydrin of the present embodiment is similar to dichloro shown in Figure 1B
The manufacturing method of propyl alcohol, below with regard to being illustrated at difference, same or similar place then repeats no more.In the dichloro third of the present embodiment
In the manufacturing method of alcohol, after carrying out step S108, it may also include and carry out step S200, step S202a and S202b.Tool
For body, while carrying out step S110a and step S110b, step S200 can be carried out, the portion of gas compressing apparatus 116 is made
The compressed product divided enters gas compressing apparatus 202 and generates compressed product.Thus, the compression of gas compressing apparatus 202
The temperature of product can also be above the temperature and pressure of the compressed product of gas compressing apparatus 116 with pressure.
Later, step S202a can be carried out, so that the compressed product of gas compressing apparatus 202 is passed through flow path P3 and is filled through heat exchange
It sets 204 and flow to phase-splitter 110.While carrying out step S202a, step S202b can be carried out, the liquid for making destilling tower 108 flow out
Body is back to destilling tower 108 by flow path P4 through heat-exchange device 204.In the present embodiment, the partially liq in destilling tower 108
It can be flowed out from the side wall of destilling tower 108, and destilling tower 108 is back to through heat-exchange device 204 by flow path P4.In other implementations
In example, the partially liq in destilling tower 108 can also be flowed out from the bottom of tower of destilling tower 108, and by flow path P4 through heat-exchange device
204 are back to destilling tower 108.The compressed product of gas compressing apparatus 202 in flow path P3 is handed over the liquid in flow path P4 in heat
Heat exchange is carried out in changing device 204.Therefore, can make to be back in destilling tower 108 after the liquid that destilling tower 108 flows out is heated,
To heat destilling tower 108.On the other hand, the temperature of the compressed product of gas compressing apparatus 202 can be reduced, then it is made to flow to split-phase
Device 110.In one embodiment, in phase-splitter 110, the compressed product and gas of the gas compressing apparatus 116 after heat exchange
The compressed product of compression set 202 forms water-phase product and includes the organic phase product of dichlorohydrin.Step is carried out in selection
In the embodiment of S106, the overhead product of the part of destilling tower 108 enters in phase-splitter 110 and is formed the water phase of phase-splitter 110
A part for product and organic phase product.In one embodiment, if after the compressed product progress heat exchange of gas compressing apparatus 202
Total condensation is not low temperature liquid, then enters back into phase-splitter 110 after it can be made to be condensed along the condensed devices 114 of flow path P3.
In other embodiment, if gas compressing apparatus 202 compressed product carry out heat exchange after can total condensation be low temperature liquid, can
It is flowed directly to phase-splitter 110 without condenser 114.
In the present embodiment, by the way that two gas compressing apparatus (gas compressing apparatus 116 and gas compressing apparatus are arranged
202) with two heat-exchange devices (heat-exchange device 118 and heat-exchange device 204), destilling tower 108 can further be reduced
Energy consumption, namely further decrease the manufacturing cost of dichlorohydrin.
Fig. 3 A and Fig. 3 B are respectively the schematic diagram of the manufacturing device of the dichlorohydrin of an embodiment and two according to the present invention
The manufacturing flow chart of chloropropyl alcohol.
Please refer to Fig. 3 A, the manufacture of the manufacturing device 300 and dichlorohydrin shown in figure 1A of the dichlorohydrin of the present embodiment
Device 100 is similar, and the manufacturing device 300 of dichlorohydrin may also include destilling tower 302.Destilling tower 108 is connected to reactor 102
Between destilling tower 302.In one embodiment, the manufacturing device 300 of dichlorohydrin may also include heat exchange pipe L, be connected to
Between the bottom of tower and the feed inlet of destilling tower 302 of destilling tower 108, so that the liquid of the bottom of tower of destilling tower 108 is along heat-exchange tube
Road L flow to the feed inlet of destilling tower 302, and the portion gas in destilling tower 302 is made to be back to destilling tower along heat exchange pipe L
108 bottom of tower.In one embodiment, whole liquid of the bottom of tower of destilling tower 108 can flow to destilling tower along heat exchange pipe L
302 feed inlet.
In one embodiment, the manufacturing device 300 of dichlorohydrin may also include phase-splitter 306, gas compressing apparatus 310 with
And heat-exchange device 312.Phase-splitter 306 can be connected to the tower top of destilling tower 302 with gas compressing apparatus 310.Heat-exchange device
312 can be connected between gas compressing apparatus 310 and phase-splitter 306 via flow path P5, and be connected to destilling tower via flow path P6
302 side wall.In addition, the manufacturing device 300 of dichlorohydrin may also include waterworks 314, it is connected directly to phase-splitter 306.
Fig. 3 A and Fig. 3 B are please referred to, the manufacturing method of the dichlorohydrin of the present embodiment is similar to dichlorohydrin shown in Figure 1B
Manufacturing method, below with regard to being illustrated at difference, same or similar place then repeats no more.In the present embodiment, in step
After S112, it may also include and carry out step S300, the liquid of the bottom of tower of destilling tower 108 is made to enter distillation along heat exchange pipe L
Tower 302, and generate overhead product and tower bottom product.In one embodiment, can make whole liquid of the bottom of tower of destilling tower 108 along
Heat exchange pipe L flow to the feed inlet of destilling tower 302.For especially, whole liquid of the bottom of tower of destilling tower 108 can be handed over along heat
The liquid flow path L1 for changing pipeline L flow to destilling tower 302.Destilling tower 302 can have reboiler 304, to provide the progress of destilling tower 302
Thermal energy needed for separation.The overhead product of destilling tower 302 is condensed rear including dichlorohydrin, and it is water-soluble to may also include hydrogen chloride
Liquid.The tower bottom product of destilling tower 302 includes a large amount of hydrochloride aqueous solutions and a large amount of catalyst, and may also include a small amount of dichlorohydrin
With a small amount of glycerine.Destilling tower 302 may include that effluent exports S2, to take out side draw product.The side draw product of destilling tower 302 includes pure
Degree is the water of 85wt% to 100wt%, and the purity of water can be 90wt% to 99.99wt% in other embodiments, most preferably
95wt% to 99.95wt%.It is similar to the side draw product for taking out destilling tower 108, is exported from effluent and takes out destilling tower 302 in S2
The reaction conversion ratio and dichlorohydrin and/or the yield of a chloropropyl alcohol of reactant also can be improved in side draw product.
Then, step S302 can be carried out, the portion gas in destilling tower 302 is made to be back to distillation along heat exchange pipe L
The bottom of tower of tower 108.For especially, above-mentioned gas has thermal energy, and can be back to steaming along the gas flow path L2 of heat exchange pipe L
Evaporate tower 108.Thus, portion gas in destilling tower 302 and in heat-exchange device 118 it is heated and be back to distillation
The gas or liquid of tower 108 can heat destilling tower 108, so that the charging of destilling tower 108 can be successfully heated and be distilled
With detach.Therefore, in the present embodiment, it can save and the cost of reboiler is set in destilling tower 108 and lowers the consumption of the energy.
Later, step S306, step S308a and step S308b can be carried out.Specifically, first carrying out step S306, make steaming
The overhead product for evaporating the part of tower 302 enters gas compressing apparatus 310 and generates compressed product.
Then step S308a is carried out, the compressed product of gas compressing apparatus 310 is made to pass through flow path P5 through heat-exchange device
312 flow to phase-splitter 306.While carrying out step S308a, step S308b is carried out, the side wall of destilling tower 302 is made to flow out
Liquid is back to destilling tower 302 by flow path P6 through heat-exchange device 312.The compression of gas compressing apparatus 310 in flow path P5
Product carries out heat exchange with the liquid in flow path P6 in heat-exchange device 312.In one embodiment, if gas compressing apparatus
310 compressed product carries out after heat exchange that total condensation is not low temperature liquid, then it can be made along the condensed devices of flow path P5 308
Phase-splitter 306 is entered back into after condensation.
While carrying out step S306, step S308a and step S308b, step S304 can be carried out, destilling tower 302 is made
The overhead product of part enter phase-splitter 306.Thus, the overhead product and gas of the destilling tower 302 in phase-splitter 306
The compressed product of body compression set 310 forms the water-phase product and organic phase product of phase-splitter 306.It in one embodiment, can be
Condenser 308 is set between the tower top and phase-splitter 306 of destilling tower 302, so that the overhead product of the part of destilling tower 302 is through cold
Phase-splitter 306 is entered back into after solidifying.
Organic phase product in phase-splitter 306 includes dichlorohydrin, and the water-phase product of phase-splitter 306 may include hydrogen chloride
Aqueous solution.In one embodiment, the water-phase product of phase-splitter 306 is reflowable to destilling tower 302.In addition, when the water of phase-splitter 306
When phase product includes hydrochloride aqueous solution, waterworks 314 can be directly connected to phase-splitter 306, directly to adjust phase-splitter
The concentration of hydrochloride aqueous solution in 306, and water-phase product is made effectively to be layered with organic product.
Then step S310 is carried out, the organic phase product in phase-splitter 306 is taken out, and obtains principal product dichlorohydrin.
In one embodiment, also the tower bottom product of destilling tower 302 can be made to be back in reactor 102, to recycle.
In the present embodiment, using in destilling tower 302 with thermal energy gas and in heat-exchange device 118 through plus
Gas that is hot and being back to destilling tower 108 or liquid heating destilling tower 108.Therefore, it can save and reboiler is set in destilling tower 108
Cost, and save the energy consumption.In addition, being to have setting gas with destilling tower 108 and destilling tower 302 in the present embodiment
Compression set with illustrate for heat-exchange device, but the present invention is not limited thereto.In other embodiments, can only exist
The one of which setting gas compressing apparatus and heat-exchange device of destilling tower 108 and destilling tower 302.
Fig. 4 A and Fig. 4 B are respectively the schematic diagram of the manufacturing device of the dichlorohydrin of an embodiment and two according to the present invention
The manufacturing flow chart of chloropropyl alcohol.
Please refer to Fig. 4 A, the manufacture of the manufacturing device 400 and dichlorohydrin shown in figure 1A of the dichlorohydrin of the present embodiment
Device 100 is similar, and the destilling tower 108 of the present embodiment may also include partition wall W.Partition wall W is extremely pushed up by the internal stretch of destilling tower 108
The top of destilling tower 108 is divided into cavity C 1 and cavity C 2 by portion.
In one embodiment, gas compressing apparatus 116 is attached to the top of cavity C 1, and heat-exchange device 118 can be through
The side wall of cavity C 1 is connected to by flow path P2.In addition, the manufacturing device 400 of dichlorohydrin may also include phase-splitter 402, gas pressure
Compression apparatus 404 and heat-exchange device 406.Phase-splitter 402 is attached to the top of cavity C 2 with gas compressing apparatus 404.Heat
Switch 406 can be connected between gas compressing apparatus 404 and phase-splitter 402 via flow path P7, and be connected by flow path P8
To the side wall of cavity C 2.It is derived from the gas of gas compressing apparatus 404 in flow path P7 and is derived from cavity C 2 in flow path P8
In liquid can carry out heat exchange in heat-exchange device 406, and then flow to phase-splitter 402 and cavity C 2 respectively.Implement one
In example, the manufacturing device 400 of dichlorohydrin may also include waterworks 408, be connected directly to phase-splitter 402.
Referring to Fig. 4 A and Fig. 4 B, the manufacturing method of the dichlorohydrin of the present embodiment is similar to dichloro shown in Figure 1B
The manufacturing method of propyl alcohol, below with regard to being illustrated at difference, same or similar place then repeats no more.The present embodiment the step of
In S104, the charging of destilling tower 108 enters cavity C 2, then past downstream to the bottom of destilling tower 108.It is flowing to destilling tower 108
The charging of bottom heated via reboiler 112 and part is evaporated, the gas of evaporation rises to cavity C 1 with cavity C 2, and is total to
The overhead product of destilling tower 108 is formed together.By destilling tower 108 bottom rise gas can with enter cavity C 2 charging into
Row heat exchange, therefore the charging for entering cavity C 2 can get thermal energy.Accordingly, the energy consumption of reboiler 112 can be reduced.In addition, destilling tower
108 may also include effluent outlet S1 exports S3 with effluent, to take out side draw product.Effluent, which exports S3, can be located at the side of cavity C 2
Wall, and effluent outlet S1 can be located at the side wall of cavity C 1.From the side of effluent outlet S1 and the destilling tower 108 of effluent outlet S3 outflows
Apoblema may include the water of purity 85% to 100%.In other embodiments, the water in the side draw product of destilling tower 108 is pure
Degree can be 90wt% to 99.99wt%, most preferably 95wt% to 99.95wt%.
In the step S106 of the present embodiment, the overhead product of the part of destilling tower 108 enters phase-splitter via cavity C 1
110.In addition, in the step S110b of the present embodiment, the liquid of the side wall outflow of the cavity C 1 of destilling tower 108 passes through flow path P2
The cavity C 1 of destilling tower 108 is back to through heat-exchange device 118.
In addition to this, after carrying out step S104, can also carry out step S402, step S404a, step S404b and
Step S406.Specifically, while carrying out step S108, step S402 can be carried out, the tower top of the part of destilling tower 108 is made
Product enters gas compressing apparatus 404 through cavity C 2, and generates compressed product.
Then, step S404a can be carried out, so that the compressed product of gas compressing apparatus 404 is passed through flow path P7 and is filled through heat exchange
It sets 406 and flow to phase-splitter 402, with the organic phase product for forming water-phase product Yu including dichlorohydrin.Carry out the same of step S404a
When, step S404b can be carried out, so that the liquid that the side wall of cavity C 2 flows out is passed through flow path P8 and is back to chamber through heat-exchange device 406
Room C2.The compressed product of gas compressing apparatus 404 in flow path P7 is carried out with the liquid in flow path P8 in heat-exchange device 406
Heat exchange.
Organic phase product in phase-splitter 402 includes dichlorohydrin, and the water-phase product of phase-splitter 402 may include hydrogen chloride
Aqueous solution.In one embodiment, the reflowable cavity C 2 to destilling tower 108 of the water-phase product of phase-splitter 402.In addition, working as split-phase
When the water-phase product of device 402 includes hydrochloride aqueous solution, waterworks 408 can be directly connected to phase-splitter 402, directly to adjust
The concentration of hydrochloride aqueous solution in whole phase-splitter 402, and water-phase product is made effectively to be layered with organic product.
While carrying out step S108 and step S402, step S400 can be carried out, the tower top of the part of destilling tower 108 is made
Product enters phase-splitter 402 through cavity C 2.Thus, which the water-phase product of phase-splitter 402 may also include steaming with organic phase product
Evaporate the overhead product of tower 108.In one embodiment, condenser 410 can be set between the top of cavity C 2 and phase-splitter 402,
So as to enter back into phase-splitter 402 after the overhead product of the part of above-mentioned destilling tower 108 is condensed.
Later, step S406 is carried out, the organic phase product in phase-splitter 402 is taken out, and obtains principal product dichlorohydrin.
In the present embodiment, the destilling tower 108 with partition wall W can be analogous to destilling tower 108 and destilling tower 302 in Fig. 3 A
In conjunction with.Specifically, the top of the destilling tower 108 of Fig. 3 A, destilling tower 302 and the bottom of destilling tower 302 can be sequentially analogous to
The bottom of cavity C 2, cavity C 1 and destilling tower 108 in Fig. 4 A.In the embodiment as shown in fig. 3 a, the bottom of destilling tower 302
Liquid it is heated and evaporate, the portion gas of evaporation rises to the top of destilling tower 302, and portion gas is along heat-exchange tube
Road L is back to destilling tower 108, to heat the charging of destilling tower 108.Similarly, in the embodiment shown in Fig. 4 A, destilling tower
The liquid of 108 bottom is heated and part is evaporated, and the portion gas of evaporation rises to cavity C 1, and on the gas of another part
Cavity C 2 is risen to heat the charging into cavity C 2.In other words, destilling tower 108 shown in Fig. 4 A be similar to will be shown in Fig. 3 A
Destilling tower 108, heat exchange pipe L and destilling tower 302 are integrated, and to carry out heat exchange, therefore can reduce manufacturing cost.
In the present embodiment, be by cavity C 1 and cavity C 2 be respectively connected with gas compressing apparatus with for heat-exchange device into
Row explanation, but the present invention is not limited thereto.In other embodiments, only cavity C 1 and the one of which of cavity C 2 is connected with
Gas compressing apparatus and heat-exchange device.
Fig. 5 A and Fig. 5 B are respectively the schematic diagram of the manufacturing device of the dichlorohydrin of an embodiment and two according to the present invention
The manufacturing flow chart of chloropropyl alcohol.
Please refer to Fig. 5 A, the manufacture of dichlorohydrin shown in manufacturing device 500 and Fig. 4 A of the dichlorohydrin of the present embodiment
Device 400 is similar, and the manufacturing device 500 of the dichlorohydrin of the present embodiment may also include gas compressing apparatus 502 and heat exchange
Device 504.Gas compressing apparatus 116 is connected between the tower top of destilling tower 108 and gas compressing apparatus 502.Heat-exchange device
504 are connected to via flow path P9 between gas compressing apparatus 502 and phase-splitter 110, and are connected to destilling tower via flow path P10
108.In the present embodiment, heat-exchange device 504 can be connected to the side wall of destilling tower 108 via flow path P10.In other embodiment
In, heat-exchange device 504 can also be connected to the bottom of tower of destilling tower 108 via flow path P10.It is derived from gas pressure in flow path P9
The gas of compression apparatus 502 can carry out heat with the liquid from destilling tower 108 in flow path P10 in heat-exchange device 504
It exchanges, and can then flow to phase-splitter 110 and destilling tower 108 respectively.
Referring to Fig. 5 A and Fig. 5 B, the manufacturing method of the dichlorohydrin of the present embodiment is similar to dichloro shown in Fig. 4 B
The manufacturing method of propyl alcohol, below with regard to being illustrated at difference, same or similar place then repeats no more.In the dichloro third of the present embodiment
In the manufacturing method of alcohol, after carrying out step S108, it may also include and carry out step S500, step S502a and step S502b.
Specifically, while carrying out step S110a and step S110b, step S500 is carried out, gas compressing apparatus is made
The compressed product of 116 part enters gas compressing apparatus 502 and generates compressed product.Thus, gas compressing apparatus 502
Compressed product temperature and pressure can also be above gas compressing apparatus 116 compressed product temperature and pressure.
Later, step S502a is carried out, the compressed product of gas compression product 502 is made to pass through flow path P9 through heat-exchange device
504 flow to phase-splitter 110.While carrying out step S502a, step S502b is carried out, keeps the liquid that destilling tower 108 flows out logical
It crosses flow path P10 and is back to destilling tower 108 through heat-exchange device 504.In the present embodiment, the partially liq in destilling tower 108 can
Side wall outflow from 1 lower section of cavity C of destilling tower 108, and destilling tower is back to through heat-exchange device 504 by flow path P10
108.In other embodiments, the partially liq in destilling tower 108 can also be flowed out from the bottom of tower of destilling tower 108, and pass through flow path
P10 is back to destilling tower 108 through heat-exchange device 504.The compressed product and flow path of gas compressing apparatus 502 in flow path P9
Liquid in P10 carries out heat exchange in heat-exchange device 504.Therefore, can make to return after the liquid that destilling tower 108 flows out is heated
It flow in destilling tower 108, to heat destilling tower 108.On the other hand, the temperature of the compressed product of gas compressing apparatus 502 can be reduced
Degree, then it is made to flow to phase-splitter 110.In one embodiment, in phase-splitter 110, the gas compressing apparatus 116 after heat exchange
The compressed product of compressed product and gas compressing apparatus 502 form water-phase product and include the organic phase product of dichlorohydrin.
In the embodiment that selection carries out step S106, the overhead product of the part of destilling tower 108 enters in phase-splitter 110 and is formed and divided
The water-phase product of phase device 110 and a part for organic phase product.In one embodiment, if the compression production of gas compressing apparatus 502
Object carries out after heat exchange that total condensation is not low temperature liquid, then after it can be made to be condensed along the condensed devices 114 of flow path P9 again into
Enter phase-splitter 110.In other embodiments, if the compressed product of gas compressing apparatus 502 can total condensation after carrying out heat exchange
For low temperature liquid, then phase-splitter 110 can be flowed directly to without condenser 114.
In addition, in the present embodiment, it is (as shown in Figure 4 A with heat-exchange device that cavity C 2 can be not connected with gas compressing apparatus
Gas compressing apparatus 404 and heat-exchange device 406).It in other words, can in the manufacturing method of the dichlorohydrin of the present embodiment
It does not select to carry out step S402 as shown in Figure 4 B, step S404a and step S404b.However, technical staff in fields
At least one of cavity C 1 and cavity C 2 can be made to be connected with an at least gas compressing apparatus according to process requirement to hand over at least one heat
Changing device, the present invention is not limited thereto.
In conclusion taking out dichlorohydrin by phase-splitter separating azeotrope, additional addition extractant is can avoid, and can
Reduce the manufacturing cost of dichlorohydrin.It forms azeotropic mixture in addition, also can avoid extractant with catalyst and catalyst is caused to be difficult to
The problem of recycling.In addition, through the compressed compressed product of gas compressing apparatus in heat-exchange device can in destilling tower
Liquid carry out heat exchange, detach required partial heat energy to provide destilling tower, and then reduce the energy consumption needed for destilling tower.
Therefore, the manufacturing cost of dichlorohydrin can further be reduced.
Although the present invention is disclosed as above with embodiment, however, it is not to limit the invention, any technical field
Middle technical staff, without departing from the spirit and scope of the present invention, when can make a little change with retouching, therefore the present invention protection
Subject to range ought be defined depending on claim.
Claims (25)
1. a kind of manufacturing device of dichlorohydrin, suitable for make glycerine and hydrochloride aqueous solution in the environment of there are catalyst into
Row reaction and generate dichlorohydrin, which is characterized in that the manufacturing device of the dichlorohydrin includes：
An at least reactor；
First destilling tower is connected to an at least reactor；
First phase-splitter is connected to the tower top of first destilling tower；
First gas compression set is connected to the tower top of first destilling tower；And
First heat-exchange device, via first flow path be connected to the first gas compression set and first phase-splitter it
Between, and it is connected to via second flow path the side wall of first destilling tower.
2. the manufacturing device of dichlorohydrin according to claim 1, which is characterized in that further include the first waterworks, directly
It is connected to first phase-splitter in succession.
3. the manufacturing device of dichlorohydrin according to claim 1, which is characterized in that being originated from the first flow path
Exist in the gas of the first gas compression set and the liquid from first destilling tower in the second flow path
After carrying out heat exchange in first heat-exchange device, it flow to first phase-splitter and first destilling tower respectively.
4. the manufacturing device of dichlorohydrin according to claim 1, which is characterized in that further include：
Second gas compression set, wherein the first gas compression set be connected to the tower top of first destilling tower with
Between the second gas compression set；And
Second heat-exchange device, via third flow path be connected to the second gas compression set and first phase-splitter it
Between, and it is connected to via the 4th flow path side wall or the bottom of tower of first destilling tower.
5. the manufacturing device of dichlorohydrin according to claim 4, which is characterized in that being originated from the third flow path
In the second gas compression set gas with the liquid in first destilling tower in the 4th flow path described
After carrying out heat exchange in second heat-exchange device, it flow to first phase-splitter and first destilling tower respectively.
6. the manufacturing device of dichlorohydrin according to claim 1, which is characterized in that further include after-fractionating tower, wherein
First destilling tower is connected to described between an at least reactor and the after-fractionating tower.
7. the manufacturing device of dichlorohydrin according to claim 6, which is characterized in that further include heat exchange pipe, connection
Between the bottom of tower and the feed inlet of the after-fractionating tower of first destilling tower, so that the bottom of tower in first destilling tower
Liquid the feed inlet of the after-fractionating tower is flow to along the heat exchange pipe, and make in the after-fractionating tower
Portion gas is back to the bottom of tower of first destilling tower along the heat exchange pipe.
8. the manufacturing device of dichlorohydrin according to claim 1, which is characterized in that first destilling tower include every
The top of first destilling tower is divided into first chamber and the by wall by the internal stretch of first destilling tower to top
Two chambers.
9. the manufacturing device of dichlorohydrin according to claim 8, which is characterized in that the first gas compression set connects
It is connected on the top of the first chamber, and first heat-exchange device is connected to the first chamber via the second flow path
Side wall.
10. the manufacturing device of dichlorohydrin according to claim 9, which is characterized in that further include：
Second phase-splitter is connected to the top of the second chamber；
Third gas compression set is connected to the top of the second chamber；And
Third heat-exchange device, via the 5th flow path be connected to the third gas compression set and second phase-splitter it
Between, and it is connected to via the 6th flow path the side wall of the second chamber.
11. the manufacturing device of dichlorohydrin according to claim 10, which is characterized in that be originated from the 5th flow path
In the third gas compression set gas in the 6th flow path be derived from the second chamber in liquid in institute
It states after carrying out heat exchange in third heat-exchange device, flow to second phase-splitter and the second chamber respectively.
12. the manufacturing device of dichlorohydrin according to claim 10, which is characterized in that further include：
Second gas compression set, wherein the first gas compression set be connected to the tower top of first destilling tower with
Between the second gas compression set；And
Second heat-exchange device, via third flow path be connected to the second gas compression set and first phase-splitter it
Between, and it is connected to via the 4th flow path side wall or the bottom of tower of first destilling tower.
13. the manufacturing device of dichlorohydrin according to claim 12, which is characterized in that the source in the third flow path
From the gas in the second gas compression set with the liquid in first destilling tower in the 4th flow path in institute
It states after carrying out heat exchange in the second heat-exchange device, flow to first phase-splitter and first destilling tower respectively.
14. the manufacturing device of dichlorohydrin according to claim 1, which is characterized in that first destilling tower includes the
Side outflux, to take out the first side draw product, first side draw product includes the water of purity 85% to 100%.
15. a kind of manufacturing method of dichlorohydrin, suitable for making glycerine with hydrochloride aqueous solution in the environment of there are catalyst
It is reacted and generates dichlorohydrin, which is characterized in that the manufacturing method of the dichlorohydrin includes：
In an at least reactor, glycerine is made to be reacted in the environment of there are catalyst with hydrochloride aqueous solution, and generated
Initial product；
So that the from the initial product first charging is entered the first destilling tower for being connected with the first phase-splitter, and generates first
Overhead product and the first tower bottom product；
First overhead product of part is set to enter first gas compression set and generate the first compressed product；
So that first compressed product is passed through first flow path and flow to first phase-splitter through the first heat-exchange device, with described
The first water-phase product is formed in first phase-splitter and includes the first organic phase product of dichlorohydrin；
So that the liquid that the side wall of first destilling tower flows out is passed through second flow path and is back to institute through first heat-exchange device
The first destilling tower is stated, wherein first compressed product in the first flow path exists with the liquid in the second flow path
Heat exchange is carried out in first heat-exchange device；And
Take out first organic phase product.
16. the manufacturing method of dichlorohydrin according to claim 15, which is characterized in that further include by the first waterworks
It is directly connected to first phase-splitter.
17. the manufacturing method of dichlorohydrin according to claim 15, which is characterized in that further include make part described
One overhead product enters first phase-splitter, wherein first overhead product in first phase-splitter and described the
One compressed product forms first water-phase product and first organic phase product.
18. the manufacturing method of dichlorohydrin according to claim 15, which is characterized in that further include：
First compressed product of part is set to enter second gas compression set and generate the second compressed product；
So that second compressed product is passed through third flow path and flow to first phase-splitter through the second heat-exchange device, wherein in institute
State first compressed product in the first phase-splitter and second compressed product formed first water-phase product with it is described
First organic phase product；And
The liquid of the side wall or bottom of tower outflow that make first destilling tower passes through the 4th flow path and is returned through second heat-exchange device
It is flow to first destilling tower, wherein
Second compressed product in the third flow path is handed over the liquid in the 4th flow path in second heat
Heat exchange is carried out in changing device.
19. the manufacturing method of dichlorohydrin according to claim 15, which is characterized in that further include：
So that the liquid of the bottom of tower in first destilling tower is entered after-fractionating tower along heat exchange pipe, and generates the second tower top
Product and the second tower bottom product；And
The portion gas in the after-fractionating tower is set to be back to the bottom of tower of first destilling tower along the heat exchange pipe.
20. the manufacturing method of dichlorohydrin according to claim 15, which is characterized in that first destilling tower include every
The top of first destilling tower is divided into first chamber and the by wall by the internal stretch of first destilling tower to top
Two chambers.
21. the manufacturing method of dichlorohydrin according to claim 20, which is characterized in that first overhead product is from institute
It states first chamber and enters first phase-splitter, and the liquid flowed out from the side wall of the first chamber passes through the second flow path
It is back to the first chamber through first heat-exchange device.
22. the manufacturing method of dichlorohydrin according to claim 21, which is characterized in that further include：
First overhead product of part is set to enter third gas compression set from the second chamber and generate third compression
Product；And
So that the third compressed product is passed through the 5th flow path and flow to the second phase-splitter through third heat-exchange device, and described second
The second water-phase product is formed in phase-splitter and includes the Second Organic Phase product of dichlorohydrin；
So that the liquid flowed out from the side wall of the second chamber is passed through the 6th flow path and is back to institute through the third heat-exchange device
Second chamber is stated, wherein the third compressed product in the 5th flow path and the liquid in the 6th flow path are in institute
It states and carries out heat exchange in third heat-exchange device；And
Take out the Second Organic Phase product.
23. the manufacturing method of dichlorohydrin according to claim 22, which is characterized in that further include make part described
One overhead product enters the second phase-splitter from the second chamber, wherein first tower top production in second phase-splitter
Object forms second water-phase product and the Second Organic Phase product with the third compressed product.
24. the manufacturing method of dichlorohydrin according to claim 22, which is characterized in that further include：
First compressed product of part is set to enter second gas compression set and generate the second compressed product；
So that second compressed product is passed through third flow path and flow to first phase-splitter through the second heat-exchange device, wherein in institute
State first compressed product in the first phase-splitter and second compressed product formed first water-phase product with it is described
First organic phase product；And
The liquid of the side wall or bottom of tower outflow that make first destilling tower passes through the 4th flow path and is returned through second heat-exchange device
It is flow to first destilling tower, wherein
Second compressed product in the third flow path is handed over the liquid in the 4th flow path in second heat
Heat exchange is carried out in changing device.
25. the manufacturing method of dichlorohydrin according to claim 15, which is characterized in that further include in first distillation
The first side draw product is taken out in the first effluent exit between the tower top and bottom of tower of tower, wherein first side draw product includes pure
Degree is the water of 85wt% to 100wt%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4900849A (en) * | 1988-09-09 | 1990-02-13 | Shell Oil Company | Process for the production of dichlorohydrin |
| JP2003306459A (en) * | 2002-04-18 | 2003-10-28 | Toagosei Co Ltd | Method for chlorinating 1,3-propanediol |
| CN101357880A (en) * | 2008-09-09 | 2009-02-04 | 南京工业大学 | Process and system for preparing dichloropropanol through autocatalytic reaction of glycerol and hydrogen chloride |
| CN106397122A (en) * | 2015-07-31 | 2017-02-15 | 王圣洁 | Method for preparing dichloropropanol and epichlorohydrin by using glycerol as raw material |
-
2017
- 2017-02-17 CN CN201710086228.0A patent/CN108456131A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4900849A (en) * | 1988-09-09 | 1990-02-13 | Shell Oil Company | Process for the production of dichlorohydrin |
| JP2003306459A (en) * | 2002-04-18 | 2003-10-28 | Toagosei Co Ltd | Method for chlorinating 1,3-propanediol |
| CN101357880A (en) * | 2008-09-09 | 2009-02-04 | 南京工业大学 | Process and system for preparing dichloropropanol through autocatalytic reaction of glycerol and hydrogen chloride |
| CN106397122A (en) * | 2015-07-31 | 2017-02-15 | 王圣洁 | Method for preparing dichloropropanol and epichlorohydrin by using glycerol as raw material |
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Effective date of registration: 20200715 Address after: 101, Section 2, Guangfu Road, Hsinchu, Taiwan, China Applicant after: Wang Shengjie Applicant after: CHANG CHUN PLASTICS Co.,Ltd. Applicant after: Chang Chun Petrochemical Co.,Ltd. Address before: No. 101, Section 2, Guangfu Road, Xinzhu City Applicant before: Wang Shengjie |
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Application publication date: 20180828 |