CN107698446A - A kind of automatic production method of the pentanediol mono isobutyrate of 2,2,4 trimethyl 1,3 - Google Patents
A kind of automatic production method of the pentanediol mono isobutyrate of 2,2,4 trimethyl 1,3 Download PDFInfo
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- CN107698446A CN107698446A CN201710834895.2A CN201710834895A CN107698446A CN 107698446 A CN107698446 A CN 107698446A CN 201710834895 A CN201710834895 A CN 201710834895A CN 107698446 A CN107698446 A CN 107698446A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07C67/00—Preparation of carboxylic acid esters
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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Abstract
The present invention relates to a kind of automatic production method of the pentanediol mono isobutyrate of 2,2,4 trimethyl 1,3, the use of liquid sodium hydroxide is catalyst, raw material isobutylaldehyde generates finished product 2 in the presence of catalyst, by reaction, the pentanediol mono isobutyrate of 2,4 trimethyl 1,3；The present invention is according to raw material and the flow and both ratios of catalyst, the residence time of material in a kettle, the temperature setting at each control point and regulatory process in flow, and the subsequent treatment of product, there is provided the continous way production technology of complete set, and use Automated condtrol.The present invention, as main reactor, realizes the automation of production process using two reactors of series connection.Not only production efficiency is high for this technique, and operation realizes automation, is advantageous to steady production and energy-saving and emission-reduction, and effective and convenient regulation can be carried out to the conversion ratio of reaction mass and actual yield.
Description
Technical field
The invention belongs to organic chemical synthesis technical field, specifically with isobutylaldehyde base catalyst effect
Under, prepare with scale 2,2, the method for 4- trimethyl -1,3- pentanediol mono isobutyrates.
Background technology
2,2,4- trimethyl -1,3- pentanediol mono isobutyrates are that the film forming of aqueous architectural coating (being usually emulsion paint) helps
Agent, there is excellent filming function, nontoxic, suitable for vinylacetate homopolymerization and copolymer emulsion, acrylate
Homopolymerization and copolymer emulsion, styrene/methacrylic acid ester copolymer emulsion, etc. multiple coating system.It is also used as water-based ink
Coalescents.Architectural Paint in China is produced per year up to 2,800,000 tons at present, and China produces more than 1000 tons building coating manufacturing enterprises per year
Account for 80%.Water emulsion coating as one of ornament materials has turned into the material of main part of inner wall of building decoration, in decoration of exterior wall
In application account for more than 60%.The alternative other poisonous coalescents of 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates,
Dosage in water emulsion coating is generally 2~6%, thus the industrialization of the coalescents have important economic implications and
Wide application prospect.The product is also a kind of important fine-chemical intermediate simultaneously, is widely used in industrial PVC plasticising
The relevant industries such as agent, lubricant.
1,3 1 pentanediols and their monoesters product such as 2,2,4- trimethyls -1,3- pentanediol lists are prepared from isobutylaldehyde aldehyde
Isobutyrate, existing many synthetic methods.These methods mostly in the presence of a base, by the autoreactivity or condensation reaction of aldehyde and
Into.In reaction, under base catalyst effect, the proton in a molecule aldehyde is moved out of, with the carbonyl reaction in another aldehyde molecule；
The alcohol aldehyde of formation, then reacted with the 3rd aldehyde molecule, produce the trimer of aldehyde, that is, described monoesters product and its accessory substance two
Alcohol.
Typical preparation technology is elaborated in following patent:US 4 225 726,US 4 883 906,DE 3
447 029 and US 5 180 847.Catalyst includes sodium hydroxide, alkaline earth metal hydroxide, stannous oxide, is all in a step
Carried out on the basis of method condensation reaction, purpose product can be obtained substantially under certain condition.
The technique isobutylaldehyde conversion rate that above-mentioned technique has many shortcomings, especially German patent DE 3 403 6 to introduce is low,
Substantial amounts of accessory substance, and complex technical process, including high pressure and two distinct types of catalyst system, product are formed in reaction
Yield at most only 40%.The technical process that CN 1098712A are introduced needs to stand point water and water-washing process twice, prepares step
Rapid more, although reaction yield can reach 69%, reaction selectivity is low, still there is considerable amount of 2,2,4 one trimethyls -1,3 one penta
The generation of diol by-product.The preparation technology first step isobutylaldehyde conversion rate 60%-95% that WO 98/24752 is described, second step
The 4- alcohol conversions of 2,6 1 diisopropyl, one 5,5 one dimethyl, one 1,3- dioxas one are 70%-75%, and accessory substance glycol contains
Amount is can be controlled within 10%, but the reaction time is extended to more than 24h to improve selectivity of product；React intermediate steps
More, it is necessary to wash stratification steps for 3 times, while need two kinds of different catalyst systems.
In recent years, it is domestic also to there is patent to propose using catalyst fixed bed, composition 2,2,4- trimethyls -1,3- penta 2 of production
The production technology of the serialization of alcohol mono isobutyrate.This technique set typically can only as the experimental rig of laboratory scale,
Used as experimental study, to be really used as industrialized production, regardless of last result, to establish such industry makeup
Put, it is also necessary to complete substantial amounts of basic work.
The content of the invention
For above-mentioned the shortcomings of the prior art, the invention discloses a kind of 2,2,4- trimethyl -1,3- pentanediol lists
The automatic production method of isobutyrate, the use of liquid sodium hydroxide is catalyst, raw material isobutylaldehyde in the presence of catalyst,
Trimethyl -1, the 3- pentanediol mono isobutyrate of finished product 2,2,4- is generated by reaction, and realizes industrialized production.
For achieving the above object, technical scheme provided by the invention is：
The automatic production method of one kind 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates, uses liquid hydroxide
Sodium is catalyst, and raw material isobutylaldehyde generates trimethyl -1, the 3- pentanediol of finished product 2,2,4- in the presence of catalyst, by reaction
Mono isobutyrate；It is the residence time of material in a kettle, each in flow by the flow of raw material and catalyst and both ratios
The temperature setting at control point and regulatory process, and the subsequent treatment of product, there is provided the continous way production technology of complete set；
All influence factors of production are systematically considered, on the basis of abundant optimization, production technology and each production are set
Parameter, Automated condtrol is used, ensured that the production technology of optimization is accurately performed and kept, ensured turning for production process
The stabilization of rate, yield and throughput rate and optimization.
The automatic production method of described 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates includes following operation and walked
Suddenly：
The first step, raw material isobutylaldehyde and catalyst alkali lye initially enter the first tank reactor in the ratio of setting, occur
Aldol reaction, the reaction temperature in the first tank reactor are set between 20~60 DEG C, former based on catalyst charge
Expect the 1-3% of quality, the residence time is set as 60 minutes；With the temperature of the tank reactor of cooling water control first；
Second step, the aldol condensate obtained by the first tank reactor enter the second tank reactor, and molecule occurs
Interior Cannizzaro is reacted, and the reaction temperature in the second tank reactor is set between 50--90 DEG C, catalyst charge
For the 1-4% of main material quality, the residence time is set as 90 minutes；Heated using steam, control the temperature of reactor；Second
Part light component gasification is had in tank reactor, its liquefaction is made by condenser, partial condensation liquid backflow auxiliary controls temperature,
A part is returned in first reactor, continues to participate in reaction；
3rd step, the material come out from the second tank reactor is semi-finished product, passes through washing, Removal of catalyst first；So
After be dehydrated, by rectifying, obtain trimethyl -1, the 3- pentanediol mono isobutyrate of finished product 2,2,4-.
The automatic control process of production process includes：
1) residence time of the inlet amount control material of isobutylaldehyde in a kettle is utilized, while utilizes the charging of isobutylaldehyde
The addition of amount control catalyst.
2) under the stable state after debugging, the conversion ratio of material and the operating mode of the yield of product and reactive moieties are pair
Answer, according to produce reality, control raw material isobutylaldehyde and product selectivity.
The water content that dehydrating tower jointly controls dehydrating prods using vacuum and temperature is less than 1%；Rectifying column utilizes vacuum
Degree, temperature and backflow；Jointly control process conditions, ensure the content of product.
The starting point of the present invention is to establish a set of industrialized process units, should disclosure satisfy that large-scale industrial production
Needs, can with security and stability produce, the conversion ratio of production process and actual yield, also disclosure satisfy that industrialized again
It is required that.
1. the basis of the present invention considers it is that production process makes every effort to easy, it to be easy to control, production capacity power is big, therefore, from
Catalyst of the liquid sodium hydroxide as reaction.This catalyst activity is high, reaction is fast, post processing is also more convenient.
2. the use of liquid sodium hydroxide being catalyst, a distinct issues are that generally, the yield of product compares
It is low, then the present invention technique setting on, selected the course of reaction of stepped serialization so that local reaction quickly,
Compare acutely.But on the overall process of production, reaction is than shallower, and so, the control to reaction is also easier
Realize accurate control.
3. in the setting of specific technique, main production process of the invention is divided into three parts, and one, two parts are synthesis
Part, Part III are product separation and purification part：
Part I, it is aldol reaction part, is carried out in the first tank reactor, reaction condition, which controls, to be compared
Gently, higher reaction selectivity is kept, while discharges the reaction heat of part, temperature is set between 20--60 DEG C, is used
20% liquid sodium hydroxide is the 1-3% of main material as catalyst, catalyst charge, and the residence time is set as 40 points
Clock.On the basis of the addition of raw material isobutylaldehyde, the addition of catalyst and the temperature of reactor are controlled.
Part II, it is Cannizzaro (Cannizzaro) reactive moieties, is carried out in the second tank reactor, reacts bar
Part controls must be than stronger, the higher reaction conversion ratio of holding.In this process, reaction discharges substantial amounts of reaction heat, profit
Jointly control the temperature of reaction with steam and with the isobutylaldehyde of backflow, temperature is set between 50--90 DEG C, uses 30% liquid
Body sodium hydroxide is the 1-4% of main material as catalyst, catalyst charge, and the residence time is set as 90 minutes.With raw material
On the basis of the addition of isobutylaldehyde, the addition of catalyst is controlled.
Part III is the last handling process of intermediate products, the intermediate material come out by reactor, by washing, is dehydrated
And obtain finished product after rectifying：
1) full gear process
The intermediate products for synthesizing later are pumped into dealdehyder tower, pass through tube still heater thing in steam slowly heating kettle
Material, while vacuum state is slowly set up, keep processing procedure smooth sequential.After starting discharging, by condensation, unreacted is reclaimed
Isobutylaldehyde.Reach -0.09 atmospheric pressure in vacuum, temperature stabilization controls 130 DEG C or so.Returned after the cooling of tower top material into raw material
With.Kettle material enters water scrubber；
2) washing step
The later material of full gear enters water scrubber, and washings enter in tower from tower top, and material enters scrubbing tower from tower bottom
It is interior, and washings reverse movement, washed.Scattered guiding device is provided with tower；
After washing terminates, material is added into dehydrating tower, under vacuo heating dehydration, control vacuum is in -0.09 air
Pressure, bottom temperature are controlled at 130 DEG C, stably continuous operation.Tower reactor discharging enters rectification working process；
3) rectification working process
Material after washing and dehydration enters rectifying double tower system, and control vacuum is in -0.09 atmospheric pressure, tower reactor temperature
At 150 DEG C, tower removing heavy constituent, two towers remove light component for degree control；Obtain finished product 2,2,4- trimethyl -1,3- pentanediol lists
Isobutyrate, content is more than 99%.
The present invention has the advantages that compared to prior art：
The invention discloses a kind of automatic production method of 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates, make
It is catalyst with liquid sodium hydroxide, raw material isobutylaldehyde generates the front three of finished product 2,2,4- in the presence of catalyst, by reaction
Base -1,3- pentanediol mono isobutyrates.The present invention is by the flow of raw material and catalyst and both ratios, and material is in a kettle
Residence time, the temperature setting at each control point and regulatory process in flow, and the subsequent treatment of product, there is provided a set of complete
Whole automatic production process.The technique invented is connected using two tank reactors, and raw material isobutylaldehyde and catalyst are pressed
The ratio of setting initially enters First reactor, and aldol reaction occurs, and the aldol condensate then obtained enters second
Platform tank reactor, the Cannizzaro reactions of intramolecular occur, successive reaction generates target product under Automated condtrol.This
Invention, as main reactor, realizes the automation of production process using two reactors of series connection.This technique is not only production effect
Rate is high, and operation realizes automation, is advantageous to steady production and energy-saving and emission-reduction, it is often more important that can be to reaction mass
Conversion ratio and actual yield carry out effective and convenient regulation, realize 2,2,4- trimethyl -1,3- pentanediol list isobutyls
The idealization production of acid esters.
Brief description of the drawings
Fig. 1：The process unit structural representation of the present invention.
Embodiment
With reference to specific embodiment, the invention will be further described.
The automatic production method of one kind 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates, use liquid hydroxide
Sodium is catalyst, and raw material isobutylaldehyde generates trimethyl -1, the 3- pentanediol of finished product 2,2,4- in the presence of catalyst, by reaction
Mono isobutyrate；It is the residence time of material in a kettle, each in flow by the flow of raw material and catalyst and both ratios
The temperature setting at control point and regulatory process, and the subsequent treatment of product, there is provided the continous way production technology of complete set,
And Automated condtrol is used.
The technological reaction device is systematically to consider all influence factors of production, on the basis fully optimized
On, production technology and each manufacturing parameter are set, Automated condtrol has been used, has ensured that the production technology of optimization is accurately held
Row and holding, ensure the conversion ratio of production process, the stabilization and optimization of yield and throughput rate.
Used process unit includes the first tank reactor, the second tank reactor, dehydrating tower, rectifying column.It is described
The first tank reactor be in series with the second tank reactor；The first tank reactor top is provided with reaction raw materials import
With the first lye import, the outlet of bottom first reactor；The second tank reactor top is provided with to be exported with first reactor
Connected pipeline and the second lye import, bottom export provided with second reactor；First tank reactor, the second autoclave are anti-
Device is answered to be provided with cooling water circulation pipeline；First flowmeter is provided with reaction raw materials entrance, in the first tank reactor, second
The pipeline being connected between tank reactor is provided with second flowmeter.
Condenser is provided with the second tank reactor top, bottom is provided with export of goods in process of manufacture, the condenser connection gas-liquid
Separator.Into the gas-liquid separation device material after separation, be partly into the second tank reactor continue it is anti-
Should, a part returns to the first tank reactor secondary response again.From the second tank reactor output semi-finished product enter back into dehydrating tower,
Rectifying column etc. is further reacted.
The automatic control process of production process includes：
1) residence time of the inlet amount control material of isobutylaldehyde in a kettle is utilized, while utilizes the charging of isobutylaldehyde
The addition of amount control catalyst.
2) under the stable state after debugging, the conversion ratio of material and the operating mode of the yield of product and reactive moieties are pair
Answer, according to produce reality, the conversion ratio for controlling raw material isobutylaldehyde is more than 80%, the selectivity control of product 95% with
On.
The water content that dehydrating tower jointly controls dehydrating prods using vacuum and temperature is less than 1%；Rectifying column utilizes vacuum
Degree, temperature and backflow；Jointly control process conditions, ensure the content of product more than 99%.
Embodiment includes as follows：
The equipment for implementing the present invention is set, according to process chart, set up device：
The stainless steel cauldron for being one cube from a volume is the first tank reactor and two cubes of a volume
Stainless steel reactor is the second tank reactor；
Dealdehyder tower, 600 millimeters of diameter, 12 meters of tower height, built-in two layers of 3 meters high of stainless steel cloth fillers；
Water scrubber, 500 millimeters of diameter, 12 meters of tower height, built-in two layers of 3 meters high of stainless steel corrugated plate packings；
Dehydrating tower, 600 millimeters of diameter, 9 meters of tower height, built-in two layers of 3 meters high of stainless steel corrugated plate packings；
Two, rectifying column, 600 millimeters of diameter, 15 meters of tower height, built-in two layers of 4 meters high of stainless steel cloth fillers；
Supporting setting pump, valve, cooling water system, vacuum system etc. simultaneously.
Implementation process：
Embodiment 1
The experimental rig of application and construction, implement production method of the present invention,
First tank reactor operating mode：
Isobutylaldehyde inlet amount, 800 ls/h,
The addition amount of sodium hydroxide of catalyst 20%, 70 ls/h,
Reaction temperature：20--60℃；
Second tank reactor operating mode：
Isobutylaldehyde inlet amount, 800 ls/h,
The addition amount of sodium hydroxide of catalyst 30%, 150 ls/h,
Reaction temperature：40--90℃；
Result of implementation, using gas chromatograph, the first tank reactor is discharged and tested and analyzed, it is as a result as follows：
Isobutylaldehyde conversion rate, 83%.
The yield of 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates, 96.4%
Embodiment 2
The experimental rig of application and construction, implement production method of the present invention,
First tank reactor operating mode：
Isobutylaldehyde inlet amount, 700 ls/h,
The addition amount of sodium hydroxide of catalyst 20%, 70 ls/h
Reaction temperature：20--60℃
Second tank reactor operating mode：
Isobutylaldehyde inlet amount, 700 ls/h,
The addition amount of sodium hydroxide of catalyst 30%, 150 ls/h
Reaction temperature：40--90℃
Result of implementation, using gas chromatograph, the first tank reactor is discharged and tested and analyzed, it is as a result as follows：
Isobutylaldehyde conversion rate, 85%
The yield of 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates, 95.3%
It is described above, only it is presently preferred embodiments of the present invention, any formal limitation not is made to the present invention, it is any ripe
Professional and technical personnel is known, it is without departing from the scope of the present invention, real to more than according to the technical spirit of the present invention
Apply any simple modification, equivalent substitution that example made and improve etc., still fall within technical solution of the present invention protection domain it
It is interior.
Claims (5)
1. one kind 2,2, the automatic production method of 4- trimethyl -1,3- pentanediol mono isobutyrates, it is characterised in that：Use liquid
Body sodium hydroxide is catalyst, and raw material isobutylaldehyde generates trimethyl -1 of finished product 2,2,4- in the presence of catalyst, by reaction,
3- pentanediol mono isobutyrates；By the flow of raw material and catalyst and both ratios, the residence time of material in a kettle,
The temperature setting at each control point and regulatory process in flow, and the subsequent treatment of product, there is provided the continous way of complete set
Production technology；Systematically consider all influence factors of production, on the basis of abundant optimization, set production technology and
Each manufacturing parameter, has used Automated condtrol, ensures that the production technology of optimization is accurately performed and kept, and ensures production
The stabilization of the conversion ratio of process, yield and throughput rate and optimization.
2. the automatic production method of according to claim 12,2,4- trimethyl -1,3- pentanediol mono isobutyrates, its
It is characterised by：Including following operating procedure：
The first step, raw material isobutylaldehyde and catalyst alkali lye initially enter the first tank reactor in the ratio of setting, and aldol occurs
Condensation reaction, the reaction temperature in the first tank reactor are set between 20~60 DEG C, and catalyst charge is main material matter
The 1-3% of amount, residence time are set as 60 minutes；With the temperature of the tank reactor of cooling water control first；
Second step, the aldol condensate obtained by the first tank reactor enter the second tank reactor, intramolecular occur
Cannizzaro is reacted, and the reaction temperature in the second tank reactor is set between 50--90 DEG C, based on catalyst charge
The 1-4% of material quality, residence time are set as 90 minutes；Heated using steam, control the temperature of reactor；In the second autoclave
Part light component gasification is had in reactor, its liquefaction is made by condenser, partial condensation liquid, which flows back, aids in control temperature, one
Divide and return in first reactor, continue to participate in reaction；
3rd step, the material come out from the second tank reactor is semi-finished product, passes through washing, Removal of catalyst first；Then take off
Water, by rectifying, obtain trimethyl -1, the 3- pentanediol mono isobutyrate of finished product 2,2,4-.
3. the automatic production method of according to claim 12,2,4- trimethyl -1,3- pentanediol mono isobutyrates, its
It is characterised by：The automatic control process of production process includes：
1) residence time of the inlet amount control material of isobutylaldehyde in a kettle is utilized, while utilizes the inlet amount control of isobutylaldehyde
The addition of catalyst processed.
2) under the stable state after debugging, the conversion ratio of material and the operating mode of the yield of product and reactive moieties are corresponding
, according to produce reality, control raw material isobutylaldehyde and product selectivity.
4. the automatic production method of according to claim 12,2,4- trimethyl -1,3- pentanediol mono isobutyrates, its
It is characterised by：The water content that dehydrating tower jointly controls dehydrating prods using vacuum and temperature is less than 1%；Rectifying column utilizes vacuum
Degree, temperature and backflow；Jointly control process conditions, ensure the content of product.
5. the automatic production method of according to claim 12,2,4- trimethyl -1,3- pentanediol mono isobutyrates, production
For raw waste gas after deep condensation reclaims most partial materials, remaining not solidifying tail gas is sent to exhaust treatment system, collects
In be uniformly processed.
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Application publication date: 20180216 |