CN106633030A - Esterified base terminated allyl alcohol polyether with high molecular weight and narrow distribution and preparation method of esterified base terminated allyl alcohol polyether - Google Patents
Esterified base terminated allyl alcohol polyether with high molecular weight and narrow distribution and preparation method of esterified base terminated allyl alcohol polyether Download PDFInfo
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- CN106633030A CN106633030A CN201611186603.0A CN201611186603A CN106633030A CN 106633030 A CN106633030 A CN 106633030A CN 201611186603 A CN201611186603 A CN 201611186603A CN 106633030 A CN106633030 A CN 106633030A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
- C08G65/3322—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
Abstract
The invention discloses esterified base terminated allyl alcohol polyether with high molecular weight and narrow distribution and a preparation method of the esterified base terminated allyl alcohol polyether. The preparation of esterified base terminated allyl alcohol polyether comprises the following steps: allyl alcohol polyether with high molecular weight and narrow distribution is synthesized from allyl alcohol and epoxide as raw materials with a segmentation method under base catalysis, polyether is refined and then directly reacts with acetic anhydride, and the esterification terminating process is finished. Most acetic anhydride and acetic acid which is produced from reaction are removed by vacuumizing under nitrogen bubbling, then a small amount of water is added in batches, acid anhydride is decomposed into acetic acid, deacidification is finished in a shorter time, and damage of long-term high temperature to the unsaturation degree of polyether is avoided. The prepared allyl alcohol polyether has advantages of narrow molecular weight distribution, stable process, good repeatability and higher reaction activity.
Description
Technical field
The invention belongs to acetyl blocked polyethers synthesis technique, more particularly to a kind of HMW narrow ditribution allyl alcohol polyether
End blocking method.
Background technology
Allyl alcohol polyether is the primary raw material of synthesizing polyether modified polyorganosiloxane, is widely used as polyurethane foams stabilizers, weaving
Auxiliary agent, oil field demulsifier, coating levelling agent, defoamer, emulsifying agent etc..End capped polyether refers to that terminal hydroxyl is taken by other functional groups
The polyethers in generation, such polyethers compares hydroxy polyethers and has that chemical stability is high, frothing capacity is low, the low performance of viscosity.Hydroxyl gathers
When Si―H addition reaction is carried out, si-h bond under the catalysis of chloroplatinic acid, is also easy to crosslink reaction ether with hydroxyl, causes product to glue
Degree is raised, and affects product quality.In soft polyurethane foam foam stabilizer, the presence of hydroxyl can cause foam closed pore, therefore in order to protect
The perforate performance of card foam, the synthesis of soft bubble foam stabilizer needs the allyl alcohol end capped polyether of HMW.
Traditional base catalyzed polymerization reaction belongs to anionic reactive, and it is based on the rapid transfer of proton that chain causes and increases
, reaction proceeds to speed that later stage proton shift to macromolecular chain due to being glued by active group relative concentration step-down and system
Spend the impacts of factor such as increase and slow down, cause the conversion ratio of epoxides to reduce and rate of side reactions increase, therefore it is difficult to close
Into the high molecular weight polyether of single functionality.Numerous patent reports synthesize high molecular weight polyether using bimetallic as catalyst
Method, but the advantage of bimetallic catalyst is polymerized without the relatively low polyethers of EO or EO contents, for soft bubble foam stabilizer
Macromolecule allyl alcohol polyether typically contains 30～50% EO, using can cause molecular weight distribution wider during bimetallic polymerization, one
Quantitative sudden and violent poly- accessory substance can also affect the application performance of product.
Polyethers is completed after esterification with acetic anhydride, and the acetic anhydride of residual can poison catalysis of the platinum during Si―H addition reaction
Act on, therefore the acetic anhydride of excess must be removed totally.Patent CN101735444 is reported and adopts toluene for dehydrating agent, azeotropic
The method of removing acetic anhydride, the problem of this method is to need a large amount of toluene, not only affects environment, is still had after the completion of reaction few
Amount Residual Toluene, affects downstream application.Patent CN101497689 reports the addition water decomposition acetic anhydride in deacidification, leads to
Falling film evaporator removing acetic acid is crossed, to be added and obtain acetyl blocked allyl alcohol polyether after refining agent adsorption filtration.
The content of the invention
It is an object of the invention to provide a kind of acetyl blocked allyl alcohol polyether of HMW narrow ditribution and its preparation
Method, the pfpe molecule amount narrowly distributing that the method is obtained, Product Activity is good, and process is simple, reproducible, is particularly suited for height
Molecular weight allyl alcohol polyether closed-end technology.
Technical scheme is as follows：
A kind of acetyl blocked allyl alcohol polyether of HMW narrow ditribution, it has following molecular formula：
Wherein, n=20～70, m=20～70, molecular weight distribution index is D=1.01-1.12, ending ratio >=95%.
A kind of method of the acetyl blocked allyl alcohol polyether for preparing above-mentioned HMW narrow ditribution, it includes following step
Suddenly：
1. the synthesis of HMW narrow ditribution allyl alcohol polyether
A. it is equipped with the stainless steel autoclave of thermometer, pressure gauge, agitator and epoxides inlet tube in 2000ml
193 grams of allyl alcohols and 1～3 gram of catalyst alkali are added, 110～120 DEG C are warming up to after nitrogen displacement, start to be slowly introducing epoxidation
450～800 grams of thing, pressure is maintained at about 0.1MPa～0.3MPa in course of reaction, and the reaction time is about 3～4 hours, then subtracts
Pressure-off removes unreacted epoxides, and reactive material is cooled into room temperature, and discharge to obtain polyethers Polyol A, polyethers Polyol A's
Number-average molecular weight is 200～300, and molecular weight distribution index is 1.01；
B. polyethers Polyol 300 grams and 1～3 gram catalyst alkali of A is added in aforesaid reaction vessel, is heated up after nitrogen displacement
To 110～120 DEG C, start to be slowly introducing 600～800 grams of epoxides, in course of reaction pressure be maintained at about 0.1～
0.3MPa, the reaction time is about 3～4 hours, and then the unreacted epoxides of removed under reduced pressure, by reactive material room is cooled to
Temperature, discharge to obtain polyethers Polyol B, and polyethers Polyol B number-average molecular weights are 900～1000, and molecular weight distribution index is 1.02；
C. polyethers Polyol 400 grams and 1～3 gram catalyst alkali of B is added in aforesaid reaction vessel, is heated up after nitrogen displacement
To 110～120 DEG C, start to be slowly introducing 600～800 grams of epoxides, in course of reaction pressure be maintained at about 0.1～
0.3MPa, the reaction time is about 3～4 hours, and then the unreacted epoxides of removed under reduced pressure, by reactive material room is cooled to
Temperature, discharge to obtain polyethers Polyol C, and number-average molecular weight is about 2250～3000, and molecular weight distribution index is 1.05；
D. polyethers Polyol 500 grams and 1～3 gram catalyst alkali of C is added in aforesaid reaction vessel, is heated up after nitrogen displacement
To 110～120 DEG C, start to be slowly introducing 500～800 grams of epoxides, in course of reaction pressure be maintained at about 0.1～
0.3MPa, the reaction time is about 4～6 hours, and then the unreacted epoxides of removed under reduced pressure, by reactive material room is cooled to
Temperature, discharge to obtain polyethers Polyol D, and polyethers Polyol D number-average molecular weights are about 4500～7000, and molecular weight distribution index is
1.08。
2. the esterification of polyethers
Add in 1000ml is equipped with the stainless steel autoclave of thermometer, pressure gauge, agitator and epoxides inlet tube
Enter 600 grams of polyethers Polyol D and 20～30 grams of acetic anhydrides, be warming up to 100～160 DEG C after nitrogen displacement, insulation reaction 2.0～
10.0；Start vacuum, vacuumize the unnecessary acid of removing, during blast nitrogen from reactor bottom, after 2.0～4.0 hours, stop
Only vacuumize, negative pressure sucks 5～10 grams of deionized waters, after stirring 0.5～1.0 hour, vacuum depickling is started again, and from reaction
Bottom portion blasts nitrogen, sampling detection acetic anhydride residual quantity after 1.0～3.0 hours, when acetic anhydride residual quantity is more than 20ppm,
Repetition is above-mentioned to add water, stirs and vacuum pumping, when acetic anhydride residual quantity then stops vacuum, direct cooling discharge less than 20ppm
Obtain HMW narrow ditribution acetyl blocked allyl alcohol polyether, ending ratio >=95%.
Above-mentioned method, described epoxides includes one or more of oxirane, expoxy propane or epoxy butane
Mixture.
Above-mentioned method, described base catalyst include metallic sodium, metallic potassium, NaOH, potassium hydroxide, sodium methoxide,
Potassium methoxide, sodium hydride or hydrofining.
Above-mentioned method, the range of number-average molecular weight of described product is 3000～7000, preferably 4000～6000.
Above-mentioned method, it is discrete method synthesis technique, by taking 5000 molecular weight polyethers as an example, the molecular weight of first paragraph synthesis
For 300, the molecular weight of second segment synthesis is 1000, and the molecular weight of the 3rd section of synthesis is 2500, and the molecular weight of the 4th section of synthesis is
5000, the multiple that molecular weight amplifies successively decreases step by step.
Above-mentioned method, the esterification of described polyethers, it is not necessary to add any catalyst, allyl alcohol polyether and acetic acid
The mol ratio of acid anhydride is 1:1.1～2.5, the reaction time is 2.0～10.0 hours, and reaction temperature is 100～160 DEG C, nitrogen bubble
The temperature for vacuumizing depickling is 120～170 DEG C, and vacuum is 0.065～0.085MPa, vacuumizes the depickling time for 2.0～4.0
Hour.
Esterification end blocking method of the present invention, is not required to cooling, and direct negative pressure adds in batches water to be decomposed into acetic anhydride
Acetic acid, each amount of water is the 0.5%～5.0% of polyethers weight, after adding water, stirs 0.5～1.0 hour continuation vacuum and takes off
Acid, sampling detection acetic anhydride residual quantity, when acetic anhydride residual quantity then stops vacuum less than 20ppm, exceedes after 1.0～2.0 hours
20ppm then continues this operation.
The acetyl blocked allyl alcohol polyether that the present invention is prepared using segmentation base catalysis method, not only solves base catalysis and is difficult to
The problem of single functionality high molecular weight polyether is obtained, and avoids the sudden and violent poly- problem of the epoxides of bimetallic catalytic generation, weight
Renaturation is good, and the product molecular weight distribution for obtaining is narrow, and with preferable hydrosilylation activity.Using addition water in batches
Method, takes off completely by the acetic anhydride of residual is decomposed into the lower acetic acid of boiling point, the mode vacuumized only with nitrogen bubble
Except acetic acid, destruction of the long-time high-temperature vacuum to product degree of unsaturation is significantly reduced.Falling film evaporation is present invention, avoiding in addition
The vacuum equipments such as device, product is adapted to large-scale industrial production without refinement treatment, process is simple.
Specific embodiment
Below by example, the invention will be further described, but is not intended to limit protection scope of the present invention.
Embodiment 1
1. the synthesis of HMW narrow ditribution allyl alcohol polyether
A. it is equipped with the stainless steel autoclave of thermometer, pressure gauge, agitator and epoxides inlet tube in 1000ml
Add 193 grams of allyl alcohols and 2 grams of potassium hydroxide, nitrogen displacement to be warming up to 110 DEG C afterwards twice, start to be slowly introducing expoxy propane and
Mixture (the mass ratio 1 of oxirane:1) 807 grams, pressure is maintained at about 0.3MPa in course of reaction, and the reaction time is about 3～
4 hours.The unreacted epoxides of removed under reduced pressure, is then cooled to room temperature by reactive material, and discharge to obtain polyethers Polyol A, number
Average molecular weight is 300, D=1.01；
B. polyethers Polyol 300 grams and 2 grams potassium hydroxide of A, nitrogen displacement are added to rise afterwards twice in aforesaid reaction vessel
Temperature starts the mixture (mass ratio 1 for being slowly introducing expoxy propane and oxirane to 110 DEG C:1) 700 grams, press in course of reaction
Power is maintained at about 0.3MPa, and the reaction time is about 3～4 hours.The unreacted epoxides of removed under reduced pressure, then by reactive material
Room temperature is cooled to, discharge to obtain polyethers Polyol B, and number-average molecular weight is 1000, D=1.02；
C. polyethers Polyol 400 grams and 2 grams potassium hydroxide of B, nitrogen displacement are added to rise afterwards twice in aforesaid reaction vessel
Temperature starts the mixture (mass ratio 1 for being slowly introducing expoxy propane and oxirane to 110 DEG C:1) 600 grams, press in course of reaction
Power is maintained at about 0.3MPa, and the reaction time is about 3～4 hours.The unreacted epoxides of removed under reduced pressure, then by reactive material
Room temperature is cooled to, discharge to obtain polyethers Polyol C, number-average molecular weight is about 2500, D=1.05；
D. polyethers Polyol 500 grams and 2 grams potassium hydroxide of C, nitrogen displacement are added to rise afterwards twice in aforesaid reaction vessel
Temperature starts the mixture (mass ratio 1 for being slowly introducing expoxy propane and oxirane to 110 DEG C:1) 500 grams, press in course of reaction
Power is maintained at about 0.3MPa, and the reaction time is about 4～6 hours.The unreacted epoxides of removed under reduced pressure, then by reactive material
Room temperature is cooled to, discharge to obtain polyethers Polyol D, number-average molecular weight is about 5000, D=1.08.
2. the esterification of polyethers
Add in 1000ml is equipped with the stainless steel autoclave of thermometer, pressure gauge, agitator and epoxides inlet tube
Enter 600 grams of polyethers D (M=5000) and 25 grams of acetic anhydrides, 120～130 DEG C are warming up to after nitrogen displacement, insulation reaction 4 hours；Open
Dynamic vacuum, vacuumizes the unnecessary acid of removing, during blast nitrogen from reactor bottom, after 2.0 hours, stop vacuumizing, bear
Pressure 5 grams of deionized waters of suction, after stirring 0.5 hour, start again vacuum depickling, and blast nitrogen from reactor bottom, and 1.0 is little
When after sampling detection acetic anhydride residual quantity, when acetic anhydride residual quantity is more than 20ppm, repetition above-mentioned added water, stirs and vacuumized
Operation, when acetic anhydride residual quantity then stops vacuum less than 20ppm, direct cooling discharge obtains HMW narrow ditribution acetyl group envelope
End allyl alcohol polyether, ending ratio is 98.2%.
Embodiment 2
1. the synthesis of HMW narrow ditribution allyl alcohol polyether
A, b, c process such as embodiment 1；
D. polyethers Polyol 500 grams and 2 grams potassium hydroxide of C, nitrogen displacement are added to rise afterwards twice in aforesaid reaction vessel
Temperature starts the mixture (mass ratio 1 for being slowly introducing expoxy propane and oxirane to 110 DEG C:1) 800 grams, press in course of reaction
Power is maintained at about 0.3MPa, and the reaction time is about 4～6 hours.The unreacted epoxides of removed under reduced pressure, then by reactive material
Room temperature is cooled to, discharge to obtain polyethers Polyol D, number-average molecular weight is about 6500, D=1.12.
2. the esterification of polyethers
Add in 1000ml is equipped with the stainless steel autoclave of thermometer, pressure gauge, agitator and epoxides inlet tube
Enter 600 grams of polyethers D (M=6500) and 20 grams of acetic anhydrides, 120～130 DEG C are warming up to after nitrogen displacement, insulation reaction 4 hours；Open
Dynamic vacuum, vacuumizes the unnecessary acid of removing, during blast nitrogen from reactor bottom, after 2.0 hours, stop vacuumizing, bear
Pressure 5 grams of deionized waters of suction, after stirring 0.5 hour, start again vacuum depickling, and blast nitrogen from reactor bottom, and 1.0 is little
When after sampling detection acetic anhydride residual quantity, when acetic anhydride residual quantity is more than 20ppm, repetition above-mentioned added water, stirs and vacuumized
Operation, when acetic anhydride residual quantity then stops vacuum less than 20ppm, direct cooling discharge obtains HMW narrow ditribution acetyl group envelope
End allyl alcohol polyether, ending ratio is 97.5%.
Claims (6)
1. a kind of acetyl blocked allyl alcohol polyether of HMW narrow ditribution, is characterized in that：It has following molecular formula：
Wherein, n=20～70, m=20～70, molecular weight distribution index is D=1.01-1.12, ending ratio >=95%.
2. a kind of method of the acetyl blocked allyl alcohol polyether of the HMW narrow ditribution prepared described in claim 1, it is special
Levy is that it comprises the steps：
1. the synthesis of HMW narrow ditribution allyl alcohol polyether
A. add in 2000ml is equipped with the stainless steel autoclave of thermometer, pressure gauge, agitator and epoxides inlet tube
193 grams of allyl alcohols and 1～3 gram of catalyst alkali, are warming up to 110～120 DEG C after nitrogen displacement, start to be slowly introducing epoxides
450～800 grams, pressure is maintained at about 0.1MPa～0.3MPa in course of reaction, and the reaction time is about 3～4 hours, then reduces pressure
Unreacted epoxides is removed, reactive material is cooled into room temperature, discharge to obtain polyethers Polyol A, the number of polyethers Polyol A
Average molecular weight is 200～300, D (molecular weight distribution index, similarly hereinafter)=1.01；
B. polyethers Polyol 300 grams and 1～3 gram catalyst alkali of A is added in aforesaid reaction vessel, is warming up to after nitrogen displacement
110～120 DEG C, start to be slowly introducing 600～800 grams of epoxides, pressure is maintained at about 0.1～0.3MPa in course of reaction,
Reaction time is about 3～4 hours, and then the unreacted epoxides of removed under reduced pressure, by reactive material room temperature is cooled to, and is discharged
Polyethers Polyol B, polyethers Polyol B number-average molecular weight is 900～1000, D=1.02；
C. polyethers Polyol 400 grams and 1～3 gram catalyst alkali of B is added in aforesaid reaction vessel, is warming up to after nitrogen displacement
110～120 DEG C, start to be slowly introducing 600～800 grams of epoxides, pressure is maintained at about 0.1～0.3MPa in course of reaction,
Reaction time is about 3～4 hours, and then the unreacted epoxides of removed under reduced pressure, by reactive material room temperature is cooled to, and is discharged
Polyethers Polyol C, number-average molecular weight is about 2250～3000, D=1.05；
D. polyethers Polyol 500 grams and 1～3 gram catalyst alkali of C is added in aforesaid reaction vessel, is warming up to after nitrogen displacement
110～120 DEG C, start to be slowly introducing 500～800 grams of epoxides, pressure is maintained at about 0.1～0.3MPa in course of reaction,
Reaction time is about 4～6 hours, and then the unreacted epoxides of removed under reduced pressure, by reactive material room temperature is cooled to, and is discharged
Polyethers Polyol D, polyethers Polyol D number-average molecular weight is 4500～6000, D=1.08.
2. the esterification of polyethers
600 are added in 1000ml is equipped with the stainless steel autoclave of thermometer, pressure gauge, agitator and epoxides inlet tube
Gram polyethers Polyol D and 20～30 grams of acetic anhydrides, are warming up to 100～160 DEG C, insulation reaction 2.0～10.0 after nitrogen displacement；
Start vacuum, vacuumize the unnecessary acid of removing, during blast nitrogen from reactor bottom, after 2.0～4.0 hours, stop taking out
Vacuum, negative pressure sucks 12 grams of deionized waters, after stirring 0.5～1.0 hour, vacuum depickling is started again, and from reactor bottom
Nitrogen is blasted, sampling detection acetic anhydride residual quantity after 1.0～3.0 hours, when acetic anhydride residual quantity is more than 20ppm, in repetition
State and add water, stir and vacuum pumping, when acetic anhydride residual quantity then stops vacuum less than 20ppm, direct cooling discharge obtains height
Molecular weight narrow ditribution acetyl blocked allyl alcohol polyether.
3. method according to claim 2, is characterized in that：Described epoxides include oxirane, expoxy propane or
The mixture of one or more of epoxy butane.
4. method according to claim 2, is characterized in that：Described base catalyst includes metallic sodium, metallic potassium, hydroxide
Sodium, potassium hydroxide, sodium methoxide, potassium methoxide, sodium hydride or hydrofining.
5. method according to claim 2, is characterized in that：The range of number-average molecular weight of described product be 3000～
7000。
6. method according to claim 2, is characterized in that：It is discrete method synthesis technique, with several equal 5000 molecular weight polyisoprenes
As a example by ether, first paragraph synthesis number-average molecular weight be 300, second segment synthesis number-average molecular weight be 1000, the 3rd section synthesis
Number-average molecular weight is 2500, and the number-average molecular weight of the 4th section of synthesis is 5000, and the multiple that molecular weight amplifies successively decreases step by step.
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| CN109942803A (en) * | 2017-12-21 | 2019-06-28 | 江苏美思德化学股份有限公司 | A kind of esterification end-capping allyl polyethers and preparation method thereof |
| CN114276548A (en) * | 2021-11-24 | 2022-04-05 | 天津工业大学 | Polyether modified organic silicon coating leveling agent and preparation method thereof |
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| CN114276548A (en) * | 2021-11-24 | 2022-04-05 | 天津工业大学 | Polyether modified organic silicon coating leveling agent and preparation method thereof |
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