CN111004380A - Water-based polyether polyalkylene glycol for high molecular weight narrow distribution metal heat treatment and preparation method thereof - Google Patents
Water-based polyether polyalkylene glycol for high molecular weight narrow distribution metal heat treatment and preparation method thereof Download PDFInfo
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- CN111004380A CN111004380A CN201911256945.9A CN201911256945A CN111004380A CN 111004380 A CN111004380 A CN 111004380A CN 201911256945 A CN201911256945 A CN 201911256945A CN 111004380 A CN111004380 A CN 111004380A
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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
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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
- C08G65/2642—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 characterised by the catalyst used
- C08G65/2645—Metals or compounds thereof, e.g. salts
- C08G65/2648—Alkali metals or compounds thereof
Abstract
The invention relates to a high molecular weight narrow distribution water-based polyether polyalkylene glycol for metal heat treatment and a preparation method thereof, wherein the preparation method comprises the following steps: (1) taking polyhydric alcohol as a first initiator and metal alkali as a first catalyst, dehydrating, dropwise adding an epoxy compound for reaction, curing, degassing and cooling to obtain a polyalkylene glycol polyether intermediate; (2) and (2) taking the polyalkylene glycol polyether intermediate prepared in the step (1) as a second initiator, taking an alkali metal hydride as a second catalyst, dehydrating, dropwise adding an epoxy compound, curing, degassing and cooling to obtain the high-molecular-weight narrow-distribution water-based polyether polyalkylene glycol. The prepared polyalkylene glycol polyether has the number average molecular weight of 10000-50000, the molecular weight distribution coefficient MW/MN is 1.15-1.4, the molecular weight is high, the molecular weight distribution is narrow, and the corresponding kinematic viscosity at 40 ℃ can reach 15000-80000mm2The viscosity index is 400-550, the viscosity is high, and the thickening property, the shearing resistance and the viscosity-temperature performance are all excellent.
Description
Technical Field
The invention relates to the technical field of metal heat treatment, in particular to high molecular weight narrow-distribution water-based polyether polyalkylene glycol and a preparation method thereof.
Background
The metal heat treatment is a process of heating a metal or alloy workpiece in a certain medium to a proper temperature, keeping the temperature for a certain time, cooling the workpiece in different media at different speeds, and controlling the performance of the workpiece by changing the microstructure of the surface or the interior of a metal material. In the process of metal heat treatment, generally, an oily substance is used as a heat treatment medium, which is called oil-based liquid for short. However, the oil-based liquid is easy to generate a large amount of smoke when in use, pollutes the environment, is not environment-friendly and causes harm to personnel.
Polyalkylene glycol, also known as PAG (PAG), is also known as polyether synthetic oil or water-based polyether polyalkylene glycol, and is widely used in quenching oil (quench), metal working fluid (metal working fluid), food-grade lubricating oil (food-grade lubricating oil), hydraulic oil (hydralic oil) and compressor oil at present. When the aqueous polyether polyalkylene glycol is used as quenching oil, the aqueous polyether polyalkylene glycol has the advantages of good stability, relatively low oxidative degradation and aging rate, no smoke, no toxicity, no corrosion, no combustion, safe use, no environmental pollution, capability of effectively reducing cracking of workpieces and low cost. However, the existing water-based polyether polyalkylene glycol has wider molecular weight distribution, the actual molecular weight is greatly different from the designed molecular weight, and if the same viscosity is achieved, the designed molecular weight is far larger than the actual molecular weight, so that the cost is increased, various properties of the polyether are reduced, such as the reduction of viscosity index and poor viscosity-temperature performance, and when the polyether is applied to the field of quenching liquid, the low-temperature quenching speed is high, metal cracking is easily caused, and the like. In addition, the wide-distribution polyether is often accompanied by side reactions such as double bond isomerization and the like in the reaction, the color value is darker, and the quality of the polyether is seriously influenced.
Therefore, there is an urgent need in the art to develop a narrow distribution, high molecular weight, high viscosity index, high performance waterborne polyether polyalkylene glycol and a preparation method thereof.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of high molecular weight narrow distribution water-based polyether polyalkylene glycol for metal heat treatment.
The present application also aims to provide a water-borne polyether polyalkylene glycol prepared by the above preparation method.
In order to achieve the object of the present invention, the present application provides the following technical solutions.
In a first aspect, the present application provides a process for preparing an aqueous polyether polyalkylene glycol for thermal treatment of high molecular weight narrow distribution metals, characterized by comprising the steps of:
(1) taking polyhydric alcohol as a first initiator and metal alkali as a first catalyst, dehydrating, then dropwise adding an epoxy compound for reaction, and obtaining a polyalkylene glycol polyether intermediate after curing, degassing, cooling and discharging;
(2) and (2) taking the polyalkylene glycol polyether intermediate prepared in the step (1) as a second initiator, taking an alkali metal hydride as a second catalyst, dehydrating, dropwise adding an epoxy compound for reaction, curing, degassing and cooling to obtain the high-molecular-weight narrow-distribution water-based polyether polyalkylene glycol for metal heat treatment.
In one embodiment of the first aspect, the polyol in step (1) is an active hydrogen-containing alcohol compound with a functionality of 2-6, and preferably, the polyol is one of ethylene glycol, diethylene glycol, propylene glycol, glycerol, pentaerythritol, sorbitol or mannitol
In one embodiment of the first aspect, the polyether intermediate prepared in step (1) has a low molecular weight and low requirements for a catalytic system, and therefore is prepared using a conventional metal base catalyst: one of potassium hydroxide, sodium hydroxide, potassium methoxide or sodium methoxide, and in the step (1), the first catalyst accounts for 0.1-1% of the total mass of the reaction system.
In one embodiment of the first aspect, in the step (1), the mass ratio of ethylene oxide to propylene oxide is (5-7): (5-3), wherein the mass ratio of the polyhydric alcohol to the ethylene oxide is 1: (5-15).
In one embodiment of the first aspect, the temperature of the reaction in step (1) is 120-130 ℃, the reaction pressure is 0-0.3 MPa, and after the reaction is finished, the temperature and the pressure are maintained for curing, wherein the curing time is 0.5-2 hours; the degassing time is 0.5-1 h; the temperature after cooling is 50-70 ℃.
In one embodiment of the first aspect, the average molecular weight of the polyalkylene glycol polyether intermediate is from 500 to 3000.
In one embodiment of the first aspect, the high molecular weight polyether prepared in step (2) cannot meet the requirements of conventional catalysts, and therefore, an alkali metal hydride with high catalytic activity is selected: one of potassium hydride or sodium hydride, and in the step (2), the second catalyst accounts for 0.01-0.07% of the total mass of the reaction system.
In one embodiment of the first aspect, in the step (2), the mass ratio of ethylene oxide to propylene oxide is (6-9): (4-1), wherein the mass ratio of the polyalkylene glycol polyether intermediate to the ethylene oxide is 1: (5-14).
In one embodiment of the first aspect, in the step (2), before the epoxy compound is added dropwise, the dehydration temperature is 110 to 120 ℃, and the dehydration time is 1 to 2 hours.
In one embodiment of the first aspect, after the epoxy compound is added dropwise in the step (2), the reaction temperature is 80-120 ℃, the reaction pressure is 0-0.1 MPa, the reaction is finished, the temperature and the pressure are kept, and the curing time is 0.5-2 hours; the degassing time is 0.5-1 h; the temperature after cooling is 50-70 ℃.
In a second aspect, the present application also provides an aqueous polyether polyalkylene glycol for thermal treatment of high molecular weight narrow distribution metal, which is prepared by the preparation method described above, and has an average molecular weight of 10000 to 50000 and a molecular weight distribution coefficient MW/MN of 1.15 to 1.4; kinetic viscosity at 40 ℃ of 15000-2Viscosity index 400-.
Compared with the prior art, the invention has the beneficial effects that:
(1) the reaction condition is mild, easy to control, no need of post-treatment, short production period, low metal ion content, clear and bright product color and no smell.
(2) The polyalkylene glycol polyether ether prepared by the methodThe molecular weight is 10000-50000, the molecular weight distribution coefficient MW/MN is 1.15-1.4, the molecular weight is high, the molecular weight distribution is narrow, and the corresponding kinematic viscosity at 40 ℃ can reach 15000-2The viscosity index is 400-550, the viscosity is high, and the thickening property, the shearing resistance and the viscosity-temperature performance are all excellent.
Detailed Description
Unless otherwise defined, technical or scientific terms used herein in the specification and claims should have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. All numerical values recited herein as between the lowest value and the highest value are intended to mean all values between the lowest value and the highest value in increments of one unit when there is more than two units difference between the lowest value and the highest value.
While specific embodiments of the invention will be described below, it should be noted that in the course of the detailed description of these embodiments, in order to provide a concise and concise description, all features of an actual implementation may not be described in detail. Modifications and substitutions to the embodiments of the present invention may be made by those skilled in the art without departing from the spirit and scope of the present invention, and the resulting embodiments are within the scope of the present invention.
According to the defects of the prior art, the invention aims to provide a preparation method of the polyalkylene glycol for preparing the narrow-distribution high-molecular-weight water-based polyether for metal heat treatment, and the polyalkylene glycol polyether prepared by the method has higher molecular weight, narrower molecular weight distribution, clear and transparent appearance, high viscosity index, good performances such as rust resistance, thickening property, lubricating property, low foaming property, cooling speed and the like compared with the conventional polyether.
The invention realizes the preparation of the water-based polyether polyalkylene glycol for the heat treatment of the narrow-distribution high-molecular-weight metal by two steps: firstly, using polyhydric alcohol as an initiator and metal alkali as a catalyst, and dropwise adding ethylene oxide and propylene oxide to synthesize a polyalkylene glycol polyether intermediate with a lower molecular weight; and step two, the product of the step one is taken as an initiator, alkali metal hydride is taken as a catalyst, ethylene oxide and propylene oxide are dripped to react to obtain the aqueous polyether polyalkylene glycol for the narrow-distribution high-molecular heat treatment. The method specifically comprises the following steps:
(1) adding polyalcohol and metal alkali into a reaction kettle, replacing nitrogen with positive pressure and negative pressure for three times, heating to 80-110 ℃, dehydrating for 0.5-1 h, dropwise adding a mixture of ethylene oxide and propylene oxide for reaction, keeping the temperature for curing for 0.5-2 h, degassing for 0.5-1 h, and finally cooling to 50-70 ℃ for discharging to obtain a lower molecular weight water random polyether intermediate;
(2) adding the intermediate and the alkali metal hydride synthesized in the first step into a reaction kettle, replacing for three times under positive and negative pressure with nitrogen, heating to 110-120 ℃, dehydrating for 1-2 h, dropwise adding a mixture of ethylene oxide and propylene oxide to react, keeping the temperature for curing for 0.5-2 h, degassing for 0.5-1 h, finally cooling to 50-70 ℃, and discharging to obtain the aqueous polyether polyalkylene glycol for narrow-distribution high-molecular-weight metal heat treatment.
In the step (1), the polyether polyol is an active hydrogen-containing compound with a functionality f of 2-6: one of ethylene glycol, diethylene glycol, propylene glycol, glycerin, pentaerythritol, sorbitol, mannitol, and the like.
The reaction temperature in the step (1) is 120-130 ℃, and the pressure is 0-0.3 Mpa.
The average molecular weight of the waterborne random polyether intermediate obtained in the step (1) is 500-3000.
The alkaline catalyst used in the step (1) is one of potassium hydroxide, sodium hydroxide, potassium methoxide and sodium methoxide, and the content of the alkaline catalyst is 0.1-1%.
In the step (1), the mass ratio of the ethylene oxide to the propylene oxide dropwise added is (5-7): (5-3).
The reaction temperature in the step (2) is 80-120 ℃ and the pressure is 0-0.1 Mpa.
The alkali metal hydride used in the step (2) is potassium hydride or sodium hydride, and the content of the alkali metal hydride is 0.01-0.07%.
The polyether polyalkylene glycol prepared in the step (2) has an average molecular weight of 10000-50000 and a molecular weight distribution coefficient MW/MN of 1.15-1.4.
The polyether polyalkylene glycol prepared in the step (2) has a kinematic viscosity of 15000-2Viscosity index 400-
The mass ratio of the ethylene oxide to the propylene oxide dripped in the step (2) is (6-9): (4-1).
The invention can be applied to different fields by adjusting the molecular weight and the structure of the polymer, the concentration of the aqueous solution of the water-based polymer and the like, and comprises the following components: hydraulic fluid, metal working fluid, rubber demoulding lubricant, textile fiber lubricant (spinning oil) and quenching fluid. And the additive amount in the water-based functional liquid is small, the cost is low, and the economic benefit is high.
Examples
The following will describe in detail the embodiments of the present invention, which are implemented on the premise of the technical solution of the present invention, and the detailed embodiments and the specific operation procedures are given, but the scope of the present invention is not limited to the following embodiments.
Example 1
The polymerization is carried out in two steps:
(1) adding 0.8kg of diethylene glycol and 11.321g of potassium hydroxide catalyst into a reaction kettle with good drying and sealing properties, replacing nitrogen with positive pressure and negative pressure for three times, heating to 100-110 ℃, dehydrating for 0.5h, dropwise adding a mixture of 4.723kg of ethylene oxide and 2.024kg of propylene oxide, reacting at the reaction temperature of 120-130 ℃ and the pressure of 0-0.3 MPa, keeping the temperature for curing for 2h after the dropwise adding is finished, degassing for 30min, and finally cooling to 60 ℃ for discharging;
(2) adding 0.8kg of the intermediate synthesized in the first step and 4.080g of potassium hydride catalyst into a reaction kettle, replacing three times by positive and negative pressure of nitrogen, heating to 110-120 ℃ for dehydration for 1h, dropwise adding a mixture of 10.240kg of ethylene oxide and 2.560kg of propylene oxide for reaction, keeping the temperature for curing for 2h after the dropwise adding is finished, degassing for 1h, and finally cooling to 60 ℃ for discharging.
Example 2
The polymerization is carried out in two steps:
(1) adding 0.8kg of glycerol and 22.174g of potassium methoxide catalyst into a reaction kettle with good drying and sealing performance, replacing nitrogen with positive pressure and negative pressure for three times, heating to 100-110 ℃, dehydrating for 0.5h, dropwise adding a mixture of 9.788kg of ethylene oxide and 4.195kg of propylene oxide, reacting at the reaction temperature of 120-130 ℃ and the pressure of 0-0.3 MPa, keeping the temperature for curing for 2h after the dropwise adding is finished, degassing for 30min, and finally cooling to 60 ℃ for discharging;
(2) adding 0.8kg of the intermediate synthesized in the first step and 7.059g of potassium hydride catalyst into a reaction kettle with good drying and sealing properties, replacing three times by positive and negative pressure of nitrogen, heating to 110-120 ℃ for dehydration for 1h, dropwise adding a mixture of 10.654kg of ethylene oxide and 2.664kg of propylene oxide for reaction, keeping the temperature for curing for 2h after the dropwise adding is finished, degassing for 1h, and finally cooling to 60 ℃ for discharging.
Example 3
The polymerization is carried out in two steps:
(1) adding 0.8kg of pentaerythritol and 26.441g of potassium methoxide catalyst into a reaction kettle with good drying and sealing performance, replacing nitrogen positive and negative pressure for three times, heating to 80-85 ℃, carrying out nitrogen blowing dehydration for 1h, dropwise adding a mixture of 11.779kg of ethylene oxide and 5.048kg of propylene oxide for reaction, keeping the temperature for curing for 2h after the dropwise adding is finished, degassing for 30min, and finally cooling to 60 ℃ for discharging;
(2) adding 0.8kg of the intermediate synthesized in the first step and 7.467g of potassium hydride catalyst into a reaction kettle with good drying and sealing properties, replacing three times by positive and negative pressure of nitrogen, heating to 110-120 ℃ for dehydration for 1h, dropwise adding a mixture of 7.893kg of ethylene oxide and 1.973kg of propylene oxide for reaction, keeping the temperature for curing for 2h after the dropwise adding is finished, degassing for 1h, and finally cooling to 60 ℃ for discharging.
The molecular weight, viscosity, etc. information for the polyether polyalkylene glycols prepared in the above examples are compared as follows:
the embodiments described above are intended to facilitate the understanding and appreciation of the application by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present application is not limited to the embodiments herein, and those skilled in the art who have the benefit of this disclosure will appreciate that many modifications and variations are possible within the scope of the present application without departing from the scope and spirit of the present application.
Claims (10)
1. A preparation method of water-based polyether polyalkylene glycol for heat treatment of high molecular weight narrow distribution metal is characterized by comprising the following steps:
(1) taking polyhydric alcohol as a first initiator and metal alkali as a first catalyst, dehydrating, then dropwise adding an epoxy compound for reaction, and obtaining a polyalkylene glycol polyether intermediate after curing, degassing, cooling and discharging;
(2) and (2) taking the polyalkylene glycol polyether intermediate prepared in the step (1) as a second initiator, taking an alkali metal hydride as a second catalyst, dehydrating, dropwise adding an epoxy compound for reaction, curing, degassing, cooling and discharging to obtain the high-molecular-weight narrow-distribution water-based polyether polyalkylene glycol.
2. The method for preparing the high molecular weight narrow distribution waterborne polyether polyalkylene glycol for heat treatment according to claim 1, wherein the polyhydric alcohol is an active hydrogen-containing alcohol compound with a functionality of 2-6, preferably one of ethylene glycol, diethylene glycol, propylene glycol, glycerol, pentaerythritol, sorbitol or mannitol.
3. The process for preparing the aqueous polyether polyalkylene glycol for thermal treatment of high molecular weight narrow distribution metal according to claim 1, wherein the metal base is one of potassium hydroxide, sodium hydroxide, potassium methoxide or sodium methoxide, and the first catalyst accounts for 0.1-1% of the total mass of the reaction system in step (1).
4. The method for preparing the waterborne polyether polyalkylene glycol for the thermal treatment of high molecular weight narrow distribution metal according to claim 1, wherein in the step (1), the mass ratio of the ethylene oxide to the propylene oxide is (5-7): (5-3), wherein the mass ratio of the polyhydric alcohol to the ethylene oxide is 1: (5-15).
5. The method for preparing the waterborne polyether polyalkylene glycol for the thermal treatment of high molecular weight narrow distribution metal according to claim 1, wherein the temperature of the reaction in the step (1) is 120-130 ℃, the reaction pressure is 0-0.3 MPa, the reaction is finished, the temperature and the pressure are kept for curing, and the curing time is 0.5-2 h; the degassing time is 0.5-1 h; and the temperature of the cooled material is 50-70 ℃.
6. The method for preparing the water-based polyether polyalkylene glycol for thermal treatment of high molecular weight narrow distribution metal according to claim 1, wherein the average molecular weight of the polyalkylene glycol polyether intermediate is 500 to 3000.
7. The process for producing the aqueous polyether polyalkylene glycol for thermal treatment of high molecular weight narrow distribution metal according to claim 1, wherein the alkali metal hydride comprises potassium hydride or sodium hydride, and in the step (2), the second catalyst accounts for 0.01 to 0.07% by mass of the total mass of the reaction system.
8. The method for preparing the waterborne polyether polyalkylene glycol for the thermal treatment of high molecular weight narrow distribution metal according to claim 1, wherein in the step (2), the mass ratio of the ethylene oxide to the propylene oxide is (6-9): (4-1), wherein the mass ratio of the polyalkylene glycol polyether intermediate to the ethylene oxide is 1: (5-14).
9. The method for preparing the waterborne polyether polyalkylene glycol for the thermal treatment of high molecular weight narrow distribution metal according to claim 1, wherein in the step (2), before the epoxy compound is added dropwise, the dehydration temperature is 110-120 ℃, and the dehydration time is 1-2 h;
after the epoxy compound is dripped, the reaction temperature is 80-120 ℃, the reaction pressure is 0-0.1 MPa, and the curing time is 0.5-2 h after the dripping is finished; the degassing time is 0.5-1 h; and the temperature of the cooled material is 50-70 ℃.
10. An aqueous polyether polyalkylene glycol for heat treatment of high molecular weight narrow distribution metal, characterized in that the polyether polyalkylene glycol is prepared by the preparation method of any one of claims 1 to 9, and the polyether polyalkylene glycol has an average molecular weight of 10000 to 50000 and a molecular weight distribution coefficient MW/MN of 1.15 to 1.4; kinetic viscosity at 40 ℃ of 15000-2Viscosity index 400-.
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