CN107400564A - Pipe reaction equipment and continuous esterification method for esterification - Google Patents
Pipe reaction equipment and continuous esterification method for esterification Download PDFInfo
- Publication number
- CN107400564A CN107400564A CN201610333830.5A CN201610333830A CN107400564A CN 107400564 A CN107400564 A CN 107400564A CN 201610333830 A CN201610333830 A CN 201610333830A CN 107400564 A CN107400564 A CN 107400564A
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- Prior art keywords
- pipe
- esterification
- kettle
- pipe reaction
- pipeline
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 124
- 238000005886 esterification reaction Methods 0.000 title claims abstract description 58
- 230000032050 esterification Effects 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 230000035484 reaction time Effects 0.000 claims abstract description 8
- 230000018044 dehydration Effects 0.000 claims description 7
- 238000006297 dehydration reaction Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000006073 displacement reaction Methods 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000002932 luster Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract description 2
- 150000002148 esters Chemical class 0.000 description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 description 6
- 235000011187 glycerol Nutrition 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 238000011017 operating method Methods 0.000 description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000021736 acetylation Effects 0.000 description 2
- 238000006640 acetylation reaction Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 1
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
- WSEFPKKOUNRCAJ-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)propane-1,3-diol;octadecanoic acid Chemical class OCC(CO)(CO)CO.CCCCCCCCCCCCCCCCCC(O)=O WSEFPKKOUNRCAJ-UHFFFAOYSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 bis- stearic acid pentaerythritol ester Chemical class 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000001119 stannous chloride Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/242—Tubular reactors in series
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/244—Concentric tubes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/02—Preparation of carboxylic acid esters by interreacting ester groups, i.e. transesterification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/06—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils with glycerol
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention relates to a kind of pipe reaction equipment and continuous esterification method for esterification, dispensing in batching kettle by with product after the heat exchange of heat exchanger coil, enable dispensing heat temperature raising, esterification is carried out subsequently into pipe reaction device, the pipe method of chuck inside and outside the use of pipe reaction device, using conduction oil as heating source, for being heated to material pipe, to reach the reaction temperature of needs, material is set successfully to carry out esterification, and caused moisture content in esterification reaction is sloughed by dehydrating kettle, indirect esterification can be carried out, the reaction of serialization can also be carried out, area occupied is small, reaction is heated evenly, improve reaction speed, shorten the reaction time, reduce energy consumption, raising to the color and luster of product is favourable, also the quality of product is just improved.
Description
Technical field
It is especially a kind of for the pipe reaction equipment of esterification and its company the present invention relates to esterification reaction equipment field
Continuous esterifying reaction method.
Background technology
Chemically said in reaction, esterification mainly includes three classes and reacted.First, ester ester exchange reaction, i.e., two kinds different
Ester generates new esters product by ester ester exchange reaction.Second, ester alcohol exchange reaction.I.e. a kind of ester swaps with a kind of alcohol
Reaction, generates new ester.Third, esterification reaction, i.e., a kind of a kind of sour and alcohol reacts, and generates ester and water.The first two kind reaction is all
Be put into how much, output is how much, does not have other products and produces.Latter reaction generation ester and water, water need to remove from reaction
Go.In existing esterification device, typically all carried out using reactor, floor space is big, and programming rate is slow, the reaction time
It is long.It also is difficult to carry out the reaction of serialization.
The content of the invention
It is an object of the invention to overcome above shortcomings in the prior art, and provide a kind of reasonable in design, structure
Simply, energy consumption is low, the efficiency high pipe reaction equipment and continuous esterification method for esterification.
Technical scheme is used by the present invention solves the above problems：A kind of pipe reaction equipment for esterification,
A kind of pipe reaction equipment for esterification, it is characterized in that including batching kettle, pipe reaction device, dehydrating kettle, finished product kettle,
Two groups of coil pipes and agitating shaft are provided with the batching kettle, the agitating shaft is located in the middle part of batching kettle, and one group of coil pipe surrounds agitating shaft
Set, another set coil pipe is set around batching kettle inwall, and two groups of coil pipes are respectively heat exchanger coil and steam pipe coil；The pipe
The pipe method of chuck inside and outside road reaction unit use, for interior conduit as material road, Outer Tube is heat-conducting oil pipes；The batching kettle
It is connected with pipe reaction device feed end pipeline, the batching kettle is connected with pipe reaction device discharge end pipeline, the dispensing
Kettle is connected with finished product kettle by pipeline, and the dehydrating kettle is connected with pipe reaction device feed end pipeline, the dehydrating kettle is with managing
Road reaction unit discharge end pipeline connection.
Dispensing is raised temperature by the present invention by steam pipe coil, dispensing is raised temperature, is carried out into pipe reaction device
Esterification, by controlling temperature, flow, the time, reach reaction completely, after pipe reaction terminates, material is passed through into dispensing
Heat exchanger coil in kettle, by carrying out heat exchange with dispensing, product is cooled, enters back into finished product kettle, carries out the shaping of product
Processing, and cause the dispensing in batching kettle to pass through the heat exchange of heat exchanger coil, heat temperature raising is obtained, takes full advantage of heat energy,
Energy consumption is reduced, realizes the reaction of serialization.
Preferably, the Outer Tube have it is a plurality of, it is parallel to be socketed on interior conduit, by handing over up and down between adjacent Outer Tube
The communicating pipe connection of mistake arrangement, using the pipe method of inside and outside chuck, for being heated to interior conduit, to reach the reaction temperature of needs
Degree, enables material successfully to carry out esterification.
Preferably, the path of the conduction oil is to enter successively from the Outer Tube at pipe reaction device discharge end
Enter, adjacent Outer Tube is entered by communicating pipe, finally flowed out from pipe reaction device feed end.
Preferably, the pipeline of the connecting pipe reaction unit feed end is provided with tee ball valve, the batching kettle, take off
The pipeline that water kettle is connected with pipe reaction device feed end is connected on tee ball valve, the batching kettle, dehydrating kettle and pipeline
Two-way valve is provided with the pipeline of reaction unit feed end connection；On the pipeline of the connecting pipe reaction unit discharge end
Provided with tee ball valve, the pipeline that the batching kettle, dehydrating kettle connect with pipe reaction device discharge end is connected in tee ball valve
On, two-way valve, the dehydrating kettle and pipeline are provided with the pipeline that the batching kettle is connected with pipe reaction device discharge end
Stop valve is provided with the pipeline of reaction unit discharge end connection.
Outer Tube of the present invention uses seamless steel pipe, and said inner tube road uses stainless steel tube, and the batching kettle, dehydrating kettle are
Stainless steel cauldron.
A kind of pipe reaction equipment for esterification carries out continuous esterification method, and its step is：
（1）Material initially enters batching kettle and carries out dispensing, needs to stir after the completion of dispensing, and slough material by pulling vacuum
In moisture content, the temperature of batching kettle is 100-150 DEG C, and the material after vacuum dehydration heats up by the heat exchanger coil of batching kettle,
Temperature of charge after heating is 150-180 DEG C；
（2）Material after heating enters pipe reaction device and carries out esterification, using conduction oil to pipeline in pipe reaction
Heating, the temperature of reacting pipe is 150-250 DEG C, and the reaction time is 30-120 minutes；
（3）The heat exchanger coil that high-temperature product after pipe reaction enters in batching kettle, by heat exchange, makes product cool
Afterwards, displacement is to the heat of heat exchanger coil simultaneously by step（1）Material after middle vacuum dehydration is heated up, the product after cooling
Pending into finished product kettle, the material after heating enters step（2）.
The temperature control of batching kettle is at 100-150 DEG C in the present invention, below, can slough less than 150 DEG C of material moisture content, with
It is normally carried out beneficial to esterification in pipeline；Pipe reaction temperature control is heated at 150-250 DEG C using conduction oil,
To control programming rate, reaction temperature and reaction time in reaction, the reaction time mainly passes through the flow velocity of material（Amount）To control.
Esterification of the present invention is carried out in the duct, it is contemplated that is had（Acid alcohol）Esterification can generate water, as
It is preferred that accessing dehydrating kettle equipment in the pipeline of esterification, it ensure that all esterifications can be adapted to enter in the present invention
OK, in step（2）In, the product of pipe reaction enters dehydrating kettle progress vacuum and sloughs caused moisture content in esterification, is dehydrated
After reenter pipe reaction device and reacted, this process is circulated until reaching being smoothed out for esterification, into step
（3）.
Enter preferably, the product of pipe reaction enters dehydrating kettle progress vacuum dehydration to pipe reaction device is reentered
The time of row reaction is 10-20 minutes.
The present invention compared with prior art, has advantages below and effect：Using pipe reaction, you can carry out indirect ester
Change reaction, the reaction of serialization can also be carried out, pipe reaction equipment can be by vertical（Or laterally）Arrangement, area occupied
Small, heat transfer is fast, and reaction is heated evenly, and improves reaction speed, shortens the reaction time, reduces energy consumption, because shortening reaction
Time, the raising to the color and luster of product is favourable, also just improves the quality of product, and the esterification with pipe reaction apparatus is anti-
It should can shorten or so 1 hour in time.
Brief description of the drawings
Fig. 1 is schematic diagram of the embodiment of the present invention.
In figure：Vacuum tube 1, batching kettle 2, pipe reaction device 3, pipe reaction device feed end 4, pipe reaction device go out
Expect end 5, dehydrating kettle 6, finished product kettle 7, heat exchanger coil 8, steam pipe coil 9, agitating shaft 11, interior conduit 12, Outer Tube 13, communicating pipe
14th, two-way valve 15, tee ball valve 16, conduction oil 17.
Embodiment
Below in conjunction with the accompanying drawings and the present invention is described in further detail by embodiment, and following examples are to this hair
Bright explanation and the invention is not limited in following examples.
Referring to Fig. 1, a kind of pipe reaction equipment for esterification, including batching kettle 2, pipe reaction device 3, dehydration
Kettle 6, finished product kettle 7, vacuum tube 1 is respectively connected with batching kettle 2, dehydrating kettle 6 and finished product kettle 7, heat exchange disk is provided with batching kettle 2
Pipe 8, steam pipe coil 9 and agitating shaft 11, agitating shaft 11 are located at the middle part of batching kettle 2, and heat exchanger coil 8 around agitating shaft 11 by setting
Put, steam pipe coil 9 is set around the inwall of batching kettle 2, and heat exchanger coil 8 and both positions of steam pipe coil 9 are in actual operating condition
Carry out interchangeable, the heat exchanger coil 8 is identical with the pipe diameter of steam pipe coil 9, and the coil diameter of the steam pipe coil 9 is big
In the coil diameter of heat exchanger coil 8.During actual installation, about at a distance of 5- between heat exchanger coil 8 and steam pipe coil 9
10cm, steam pipe coil 9 is with the inwall of batching kettle 2 at a distance of about 10cm.
The present embodiment batching kettle 2 is connected with the pipeline of pipe reaction device feed end 4, and the heat exchanger coil 8 in batching kettle 2 enters
Material end pipe mouth is connected with the pipeline of pipe reaction device discharge end 4, the discharge end mouth of pipe of heat exchanger coil 8 and finished product in batching kettle 2
Kettle 7 is connected by pipeline, and dehydrating kettle 6 is connected with the pipeline of pipe reaction device feed end 4, dehydrating kettle 6 goes out with pipe reaction device
Expect the connection of the pipeline of end 5.
The pipe method of chuck inside and outside the use of the present embodiment pipe reaction device 3, interior conduit 12 is as material road, Outer Tube
13 be heat-conducting oil pipes, and a plurality of Outer Tube 13 is parallel to be socketed on interior conduit 12, passes through upper and lower staggered row between adjacent Outer Tube 13
The communicating pipe 14 of cloth connects, and the path of conduction oil 17 is entered for the Outer Tube 13 successively from pipe reaction device discharge end 5
Enter, adjacent Outer Tube 13 is entered by communicating pipe 14, finally flowed out from pipe reaction device feed end 4.
The pipeline of connecting pipe reaction unit feed end 4 of the present invention is provided with tee ball valve 16, batching kettle 2, dehydrating kettle 6 with
The pipeline that pipe reaction device feed end 4 connects is connected on tee ball valve 16, and batching kettle 2, dehydrating kettle 6 and pipe reaction fill
Put and be provided with two-way valve 15 on the pipeline of the connection of feed end 4；The pipeline of connecting pipe reaction unit discharge end 5 is provided with three
Pass ball valve 16, the pipeline that batching kettle 2, dehydrating kettle 6 are connected with pipe reaction device discharge end 5 are connected on tee ball valve 16,
Two-way valve 15 is provided with the pipeline that batching kettle 2 is connected with pipe reaction device discharge end 5, dehydrating kettle 6 fills with pipe reaction
Put and be provided with stop valve 18 on the pipeline of the connection of discharge end 5, the setting of two-way valve 15 and tee ball valve 16 is used for control material
Flow velocity.
Continuous esterification of the present invention is further described below by embodiment.
Embodiment 1：
Ester ester exchange reaction, the single, double tristerin of acetylation produce operation.
Reaction principle：Hydrogenated oil and fat（Ester）+ triacetyl glycerine（Ester）--- → acetylation list bi-tristearin
The raw material and esterification feed of use（In molar ratio）Match and be：
Solid grease（Also known as：Hydrogenated oil and fat） 1；
Triacetyl glycerine（Also known as：Acetylated glycerol） 1.
Operating method：The hydrogenated oil and fat of fusing is sucked in batching kettle 2 with vacuum, triacetyl glycerine is then added, adds
Esterification catalyst sodium hydroxide（By the 0.4% of the total amount that feeds intake, with being added after a small amount of aqueous fusion）.Heated in batching kettle 2 with steam
120 DEG C or so are warming up to, sloughs the moisture content of fused catalyst.Esterification is carried out subsequently into pipe reaction device 3（Control thing
Material temperature degree is at 190-200 DEG C, the about 60 minutes time about reacted in the duct（Control pipeline is come with the length and flow of pipeline
Middle residence time）, from the product of pipe reaction device 3 out, heat is carried out by entering the heat exchanger coil 8 in batching kettle 2
Exchange enters finished product kettle 7, and product temperatur is down to 140-150 DEG C from 200 DEG C, and batch temperature rises to 160 DEG C from 120 DEG C.It can enter
Pipe reaction device 3 reacts.
Product index test is as follows：
Color and luster/solid (cream) body of range estimation white
Fusing point, DEG C 32.0
Free fatty, % 1.16
Iodine value, gI2/100g 0.21
Moisture content,（105 DEG C/2 hours）% 0.12
Density,（50℃） 0.998.
Embodiment 2：
Ester alcohol exchange reaction, glycerin monostearate produce operation.
Reaction principle：Hydrogenated oil and fat（Ester）+ glycerine（Alcohol）--- → mono- bi-tristearin
The raw material and esterification feed of use（In molar ratio）Match and be：
Solid grease（Also known as：Hydrogenated oil and fat） 1
Glycerine 1.5.
Operating method：The hydrogenated oil and fat of fusing is sucked in batching kettle 2 with vacuum, the glycerine measured is then added, adds
Esterification catalyst sodium hydroxide（By the 0.4% of the total amount that feeds intake, with being added after a small amount of aqueous fusion）.Heated in batching kettle 2 with steam
140 DEG C or so are warming up to, sloughs the moisture content of fused catalyst.Esterification is carried out subsequently into pipe reaction device 3（Control thing
Material temperature degree is at 200-210 DEG C, the about 40 minutes time about reacted in the duct（Control pipeline is come with the length and flow of pipeline
Middle residence time）, from the product of pipe reaction device 3 out, heat is carried out by entering the heat exchanger coil 8 in batching kettle 2
Exchange enters finished product kettle, and product temperatur is down to 140-150 DEG C from 210 DEG C, and batch temperature rises to 180 DEG C from 140 DEG C.Pipe can be entered
Road reaction unit 3 reacts.
Product index test is as follows：
Color and luster/range estimation white powder
Fusing point, DEG C 58.0
Free fatty, % 0.61
Iodine value, gI2/100g 0.38
Moisture content,（105 DEG C/2 hours）, % 0.12.
Embodiment 3：
Esterification reaction, double stearic acid pentaerythritol esters produce operation.
Reaction principle：Stearic acid（Acid）+ pentaerythrite（Alcohol）--- → bis- stearic acid pentaerythritol ester+water
The raw material and esterification feed of use（In molar ratio）Match and be：
Stearic acid 2
Pentaerythrite 1.
Operating method：Stearic acid after fusing is sucked in batching kettle 2 with vacuum, pentaerythrite is then added, adds ester
Change catalyst stannous chloride（By the 0.2% of the total amount that feeds intake, with being added after a small amount of aqueous fusion）.Heated and risen with steam in batching kettle 2
Temperature sloughs the moisture content of fused catalyst to 140 DEG C or so.Esterification is carried out subsequently into pipe reaction device 3（Control material
Temperature is at 210-220 DEG C, the about 90 minutes time about reacted in the duct（Come with the length and flow of pipeline in control pipeline
Residence time, this process include the secondary dewatering time into dehydrating kettle 6）, with what is come out from pipe reaction device 3
Product, heat exchange is carried out by the heat exchanger coil 8 entered in batching kettle 2 and enters finished product kettle, product temperatur is down to from 220 DEG C
140-150 DEG C, batch temperature rises to 190 DEG C from 140 DEG C.It can be reacted into pipe reaction device 3.
Product index test is as follows：
Color and luster/range estimation white powder
Fusing point, DEG C 57.5
Acid value, KOHmg/g 1.28
Iodine value, I2g/100g 0.32
Volatility,（2 hours/105 DEG C）, % 0.25.
The esterification carried out by the pipe reaction of the present invention, the product produced after tested, fully meet production
The physical and chemical index of product, better than the product of conventional reactor production in appearance luster.
Claims (8)
1. a kind of pipe reaction equipment for esterification, it is characterized in that：Including batching kettle, pipe reaction device, dehydrating kettle,
Finished product kettle, the batching kettle is interior to be provided with two groups of coil pipes and agitating shaft, and the agitating shaft is located in the middle part of batching kettle, and one group of coil pipe surrounds
Agitating shaft is set, and another set coil pipe is set around batching kettle inwall, and two groups of coil pipes are respectively heat exchanger coil and steam pipe coil；
The pipe method of chuck inside and outside the pipe reaction device use, for interior conduit as material road, Outer Tube is heat-conducting oil pipes；
The batching kettle is connected with pipe reaction device feed end pipeline, the batching kettle and pipe reaction device discharge end pipeline
Connection, the batching kettle are connected with finished product kettle by pipeline, and the dehydrating kettle is connected with pipe reaction device feed end pipeline, institute
Dehydrating kettle is stated to be connected with pipe reaction device discharge end pipeline.
2. the pipe reaction equipment according to claim 1 for esterification, it is characterized in that：The Outer Tube has more
Bar, it is parallel to be socketed on interior conduit, connected between adjacent Outer Tube by communicating pipe staggered up and down.
3. the pipe reaction equipment according to claim 2 for esterification, it is characterized in that：The path of conduction oil be according to
The secondary Outer Tube from pipe reaction device discharge end enters, and enters adjacent Outer Tube by communicating pipe, finally from positioned at pipe
Flowed out at road reaction unit feed end.
4. the pipe reaction equipment according to claim 1 for esterification, it is characterized in that：The connecting pipe reaction
The pipeline of device feed end is provided with tee ball valve, the pipe of the batching kettle, dehydrating kettle and the connection of pipe reaction device feed end
Road is connected on tee ball valve, is respectively provided with the pipeline of the batching kettle, dehydrating kettle and the connection of pipe reaction device feed end
There is two-way valve；The pipeline of the connecting pipe reaction unit discharge end is provided with tee ball valve, the batching kettle, dehydrating kettle with
The pipeline of pipe reaction device discharge end connection is connected on tee ball valve, the batching kettle and pipe reaction device discharge end
Two-way valve is provided with the pipeline of connection, is provided with and cuts on the pipeline that the dehydrating kettle is connected with pipe reaction device discharge end
Only valve.
5. the pipe reaction equipment according to claim 1 for esterification, it is characterized in that：The Outer Tube uses nothing
Steel pipe is stitched, said inner tube road uses stainless steel tube, and the batching kettle, dehydrating kettle are stainless steel cauldron.
6. a kind of pipe reaction equipment for esterification using described in Claims 1 to 55 carries out continuous esterification side
Method, its step are：
（1）Material initially enters batching kettle and carries out dispensing, needs to stir after the completion of dispensing, and slough material by pulling vacuum
In moisture content, the temperature of batching kettle is 100-150 DEG C, and the material after vacuum dehydration heats up by the heat exchanger coil of batching kettle,
Temperature of charge after heating is 150-180 DEG C；
（2）Material after heating enters pipe reaction device and carries out esterification, using conduction oil to pipeline in pipe reaction
Heating, the temperature of reacting pipe is 150-250 DEG C, and the reaction time is 30-120 minutes；
（3）The heat exchanger coil that high-temperature product after pipe reaction enters in batching kettle, by heat exchange, makes product cool
Afterwards, displacement is to the heat of heat exchanger coil simultaneously by step（1）Material after middle vacuum dehydration is heated up, the product after cooling
Pending into finished product kettle, the material after heating enters step（2）.
7. the pipe reaction equipment according to claim 6 for esterification carries out continuous esterification method, it is special
Sign is：In step（2）In, the product of pipe reaction enters dehydrating kettle progress vacuum and sloughs caused moisture content in esterification, takes off
Pipe reaction device is reentered after water to be reacted, and this process is circulated until reaching being smoothed out for esterification, into step
Suddenly（3）.
8. the pipe reaction equipment according to claim 7 for esterification carries out continuous esterification method, it is special
Sign is：The product of pipe reaction enters dehydrating kettle and carries out vacuum dehydration to the time for reentering pipe reaction device and being reacted
For 10-20 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610333830.5A CN107400564A (en) | 2016-05-19 | 2016-05-19 | Pipe reaction equipment and continuous esterification method for esterification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610333830.5A CN107400564A (en) | 2016-05-19 | 2016-05-19 | Pipe reaction equipment and continuous esterification method for esterification |
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| Publication Number | Publication Date |
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| CN107400564A true CN107400564A (en) | 2017-11-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610333830.5A Pending CN107400564A (en) | 2016-05-19 | 2016-05-19 | Pipe reaction equipment and continuous esterification method for esterification |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112354510A (en) * | 2020-11-16 | 2021-02-12 | 徐超 | Multi-stage tubular reactor with vertical spacing sections |
| CN115155465A (en) * | 2022-07-05 | 2022-10-11 | 嘉兴中诚环保科技股份有限公司 | Reaction kettle for improving esterification reaction yield and control method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417865A (en) * | 2010-09-28 | 2012-04-18 | 江苏中鼎化学有限公司 | Method for continuously producing mono-di-fatty glyceride |
| CN103553921A (en) * | 2013-11-20 | 2014-02-05 | 山东理工大学 | Continuous dehydration esterification reaction device as well as continuous esterification reaction method |
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2016
- 2016-05-19 CN CN201610333830.5A patent/CN107400564A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417865A (en) * | 2010-09-28 | 2012-04-18 | 江苏中鼎化学有限公司 | Method for continuously producing mono-di-fatty glyceride |
| CN103553921A (en) * | 2013-11-20 | 2014-02-05 | 山东理工大学 | Continuous dehydration esterification reaction device as well as continuous esterification reaction method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112354510A (en) * | 2020-11-16 | 2021-02-12 | 徐超 | Multi-stage tubular reactor with vertical spacing sections |
| CN115155465A (en) * | 2022-07-05 | 2022-10-11 | 嘉兴中诚环保科技股份有限公司 | Reaction kettle for improving esterification reaction yield and control method thereof |
| CN115155465B (en) * | 2022-07-05 | 2024-01-26 | 嘉兴中诚环保科技股份有限公司 | Reaction kettle for improving esterification reaction yield and control method thereof |
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Application publication date: 20171128 |