CN113667092A - Preparation method of high molecular weight polyether for memory pillow - Google Patents
Preparation method of high molecular weight polyether for memory pillow Download PDFInfo
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- CN113667092A CN113667092A CN202110962943.2A CN202110962943A CN113667092A CN 113667092 A CN113667092 A CN 113667092A CN 202110962943 A CN202110962943 A CN 202110962943A CN 113667092 A CN113667092 A CN 113667092A
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- Prior art keywords
- ether glycol
- polytetrahydrofuran ether
- heating
- molecular weight
- reaction
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a preparation method of high molecular weight polyether for a memory pillow, which comprises the following steps: putting the polytetrahydrofuran ether glycol into a dehydrator with a stirring structure, heating until the polytetrahydrofuran ether glycol is melted, starting stirring and continuing heating, vacuumizing in the heating process, dehydrating for 2 hours, cooling to 50 ℃ to obtain dry polytetrahydrofuran ether glycol, adding isophthalic acid, methanol and sulfuric acid into a reaction kettle, stirring and heating, refluxing for 20 hours, and recovering the methanol after the reaction is finished. According to the invention, the polytetrahydrofuran ether glycol and the dimethyl isophthalate are subjected to polymerization reaction, and meanwhile, isopropyl titanate is added as a catalyst for catalyzing the prepolymerization reaction of the polytetrahydrofuran ether glycol and the dimethyl isophthalate, so that the polytetrahydrofuran ether glycol and the dimethyl isophthalate can react more thoroughly, the chemical property of the synthesized polyether polyurethane can meet the requirement, the defective rate is reduced, and the working efficiency is improved.
Description
Technical Field
The invention relates to the technical field of memory pillows, in particular to a preparation method of high molecular weight polyether for a memory pillow.
Background
The memory pillow is made of a slow rebound material, the function of the memory pillow is not to increase the memory of a person but because the frequently used pillow can form the inherent shape of the head and the neck of the person, the memory pillow is mostly a slow rebound pillow, has good protection capability and excellent chemical substance resistance, is chemically inert to most of acid, alkali and salt, has good liquid blocking protection function, porous substances and good air permeability, and can not easily permeate liquid water, oil and the like due to fine and dense fibers; the gas and the water vapor can penetrate through the packaging bag, so that the packaging bag has excellent waterproof and breathable performance, good solid particle penetration prevention function and a special physical organization structure, can completely block fine mites and dust, prevents the mites and the dust from penetrating through the packaging bag, has excellent bacterium blocking effect, can be applied to packaging of sterile medical products, and is low in fluffiness, durable, free of fluffing, high in strength, excellent in size stability and easy to process.
The material of current memory pillow is polyether type polyurethane, when carrying out chemical synthesis to polyether type polyurethane, can lead to the polyether type polyurethane chemical property that the synthesis came out can't reach the requirement because the prepolymerization reaction is not thorough in the prepolymerization reaction, leads to the defective percentage higher, and work efficiency is low.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a preparation method of high molecular weight polyether for a memory pillow.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high molecular weight polyether for a memory pillow comprises the following steps:
s1: polyether dehydration: putting the polytetrahydrofuran ether glycol into a dehydrator with a stirring structure, heating until the polytetrahydrofuran ether glycol is melted, starting stirring and continuing heating at the moment, vacuumizing in the heating process, dehydrating for 2 hours, and cooling to 50 ℃ to obtain dried polytetrahydrofuran ether glycol;
s2: adding isophthalic acid, methanol and sulfuric acid into a reaction kettle, stirring and heating, refluxing for 20h, recovering methanol after the reaction is finished, neutralizing the reactant, filtering, and drying to obtain dimethyl isophthalate;
s3: putting the dried polytetrahydrofuran ether glycol into a polymerization kettle, adding dimethyl isophthalate, uniformly stirring, heating to a polymerization temperature, adding isopropyl titanate after the mixture is completely melted, adjusting to a prepolymerization pressure for prepolymerization reaction, heating to a polycondensation temperature after 1-3h, and carrying out high vacuum polycondensation reaction to obtain a molten prepolymer;
s4: and adding 10-20% by mass of 1, 4-butanediol into the molten prepolymer, putting the mixture into a forming die, and cooling to obtain the formed polyether polyurethane.
Preferably, the final temperature of the temperature rise in S1 is 110 ℃ to 120 ℃, the vacuum degree is 130Pa, the molecular weight of the polytetrahydrofuran ether glycol is 3000, and the character is white waxy solid.
Preferably, the neutralization solution in S2 is sodium carbonate solution, and the pH value after neutralization is 7-8.
Preferably, the polymerization temperature in the S3 is 75-80 ℃, and the prepolymerization pressure is 2 x 10-40.085Mpa, the polycondensation temperature is 150-200 ℃, and the high vacuum polycondensation reaction time is 1-2 h.
The invention has the beneficial effects that:
according to the invention, the polytetrahydrofuran ether glycol and the dimethyl isophthalate are subjected to polymerization reaction, and meanwhile, isopropyl titanate is added as a catalyst for catalyzing the prepolymerization reaction of the polytetrahydrofuran ether glycol and the dimethyl isophthalate, so that the polytetrahydrofuran ether glycol and the dimethyl isophthalate can react more thoroughly, the chemical property of the synthesized polyether polyurethane can meet the requirement, the defective rate is reduced, and the working efficiency is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Embodiment 1, a method for preparing high molecular weight polyether for memory pillow, comprising the following steps:
s1: polyether dehydration: putting polytetrahydrofuran ether glycol into a dehydrator with a stirring structure, heating until the polytetrahydrofuran ether glycol is melted, starting stirring and continuing heating, vacuumizing in the heating process, dehydrating for 2 hours, and cooling to 50 ℃ to obtain dry polytetrahydrofuran ether glycol, wherein the final temperature of heating is 110-120 ℃, the vacuum degree is 130Pa, the molecular weight of the polytetrahydrofuran ether glycol is 3000, and the character of the polytetrahydrofuran ether glycol is white waxy solid;
s2: adding isophthalic acid, methanol and sulfuric acid into a reaction kettle, stirring and heating, refluxing for 20h, recovering methanol after the reaction is finished, neutralizing the reactant, filtering and drying to obtain dimethyl isophthalate, wherein the neutralized solution is a sodium carbonate solution, and the pH value after neutralization is 7-8;
s3: putting dried polytetrahydrofuran ether glycol into a polymerization kettle, adding dimethyl isophthalate, uniformly stirring, heating to a polymerization temperature, adding isopropyl titanate after the mixture is completely melted, adjusting to a prepolymerization pressure for prepolymerization reaction, heating to a polycondensation temperature after 1-3h, and carrying out high vacuum polycondensation reaction to obtain a molten prepolymer, wherein the polymerization temperature is 75-80 ℃, and the prepolymerization pressure is 2 x 10-40.085Mpa, the polycondensation temperature is 150-200 ℃, and the high vacuum polycondensation reaction time is 1-2 h;
s4: and adding 10 mass percent of 1, 4-butanediol into the molten prepolymer, putting the mixture into a forming die, and cooling to obtain the formed polyether polyurethane.
Embodiment 2, a method for preparing high molecular weight polyether for memory pillow, comprising the following steps:
s1: polyether dehydration: putting polytetrahydrofuran ether glycol into a dehydrator with a stirring structure, heating until the polytetrahydrofuran ether glycol is melted, starting stirring and continuing heating, vacuumizing in the heating process, dehydrating for 2 hours, and cooling to 50 ℃ to obtain dry polytetrahydrofuran ether glycol, wherein the final temperature of heating is 110-120 ℃, the vacuum degree is 130Pa, the molecular weight of the polytetrahydrofuran ether glycol is 3000, and the character of the polytetrahydrofuran ether glycol is white waxy solid;
s2: adding isophthalic acid, methanol and sulfuric acid into a reaction kettle, stirring and heating, refluxing for 20h, recovering methanol after the reaction is finished, neutralizing the reactant, filtering and drying to obtain dimethyl isophthalate, wherein the neutralized solution is a sodium carbonate solution, and the pH value after neutralization is 7-8;
s3: putting dried polytetrahydrofuran ether glycol into a polymerization kettle, adding dimethyl isophthalate, uniformly stirring, heating to a polymerization temperature, adding isopropyl titanate after the mixture is completely melted, adjusting to a prepolymerization pressure for prepolymerization reaction, heating to a polycondensation temperature after 1-3h, and carrying out high vacuum polycondensation reaction to obtain a molten prepolymer, wherein the polymerization temperature is 75-80 ℃, and the prepolymerization pressure is 2 x 10-40.085Mpa, the polycondensation temperature is 150-200 ℃, and the high vacuum polycondensation reaction time is 1-2 h;
s4: and adding 15 mass percent of 1, 4-butanediol into the molten prepolymer, putting the mixture into a forming die, and cooling to obtain the formed polyether polyurethane.
Embodiment 3, a method for preparing high molecular weight polyether for memory pillow, comprising the following steps:
s1: polyether dehydration: putting polytetrahydrofuran ether glycol into a dehydrator with a stirring structure, heating until the polytetrahydrofuran ether glycol is melted, starting stirring and continuing heating, vacuumizing in the heating process, dehydrating for 2 hours, and cooling to 50 ℃ to obtain dry polytetrahydrofuran ether glycol, wherein the final temperature of heating is 110-120 ℃, the vacuum degree is 130Pa, the molecular weight of the polytetrahydrofuran ether glycol is 3000, and the character of the polytetrahydrofuran ether glycol is white waxy solid;
s2: adding isophthalic acid, methanol and sulfuric acid into a reaction kettle, stirring and heating, refluxing for 20h, recovering methanol after the reaction is finished, neutralizing the reactant, filtering and drying to obtain dimethyl isophthalate, wherein the neutralized solution is a sodium carbonate solution, and the pH value after neutralization is 7-8;
s3: putting dried polytetrahydrofuran ether glycol into a polymerization kettle, adding dimethyl isophthalate, uniformly stirring, heating to a polymerization temperature, adding isopropyl titanate after the mixture is completely melted, adjusting to a prepolymerization pressure for prepolymerization reaction, heating to a polycondensation temperature after 1-3h, and addingHigh vacuum polycondensation reaction to obtain molten prepolymer at 75-80 deg.c and 2X 10 pre-polymerization pressure-40.085Mpa, the polycondensation temperature is 150-200 ℃, and the high vacuum polycondensation reaction time is 1-2 h;
s4: and adding 20 mass percent of 1, 4-butanediol into the molten prepolymer, putting the mixture into a forming die, and cooling to obtain the formed polyether polyurethane.
The tensile property test and the shore a hardness test are performed on the above embodiment, the tensile property test instrument is a universal tensile testing machine, the test is performed according to GB/T528-:
| shore A hardness | Tensile strength/MPa | |
| Example 1 | 88 | 11.6 |
| Example 2 | 92 | 15.9 |
| Example 3 | 90 | 13.3 |
As can be seen from the above table, example 2 is the most preferred embodiment of the present invention.
In the description of the present invention, it is to be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," and the like are used in an orientation or positional relationship that is indicative of, or indicative of, but not limiting of, the present invention, merely for the convenience and simplicity of description, and that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. A preparation method of high molecular weight polyether for a memory pillow is characterized by comprising the following steps:
s1: polyether dehydration: putting the polytetrahydrofuran ether glycol into a dehydrator with a stirring structure, heating until the polytetrahydrofuran ether glycol is melted, starting stirring and continuing heating at the moment, vacuumizing in the heating process, dehydrating for 2 hours, and cooling to 50 ℃ to obtain dried polytetrahydrofuran ether glycol;
s2: adding isophthalic acid, methanol and sulfuric acid into a reaction kettle, stirring and heating, refluxing for 20h, recovering methanol after the reaction is finished, neutralizing the reactant, filtering, and drying to obtain dimethyl isophthalate;
s3: putting the dried polytetrahydrofuran ether glycol into a polymerization kettle, adding dimethyl isophthalate, uniformly stirring, heating to a polymerization temperature, adding isopropyl titanate after the mixture is completely melted, adjusting to a prepolymerization pressure for prepolymerization reaction, heating to a polycondensation temperature after 1-3h, and carrying out high vacuum polycondensation reaction to obtain a molten prepolymer;
s4: and adding 10-20% by mass of 1, 4-butanediol into the molten prepolymer, putting the mixture into a forming die, and cooling to obtain the formed polyether polyurethane.
2. The method for preparing the high molecular weight polyether for the memory pillow according to claim 1, wherein the final temperature of the temperature rise in the step S1 is 110-120 ℃, the vacuum degree is 130Pa, the molecular weight of the polytetrahydrofuran ether glycol is 3000, and the character is white waxy solid.
3. The method for preparing the high molecular weight polyether for the memory pillow as claimed in claim 1, wherein the neutralization solution in S2 is sodium carbonate solution, and the pH value after neutralization is 7-8.
4. The method for preparing the high molecular weight polyether for the memory pillow as claimed in claim 1, wherein the polymerization temperature in S3 is 75-80 ℃, and the prepolymerization pressure is 2 x 10-40.085Mpa, the polycondensation temperature is 150-200 ℃, and the high vacuum polycondensation reaction time is 1-2 h.
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| CN202110962943.2A CN113667092A (en) | 2021-08-20 | 2021-08-20 | Preparation method of high molecular weight polyether for memory pillow |
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| CN202110962943.2A CN113667092A (en) | 2021-08-20 | 2021-08-20 | Preparation method of high molecular weight polyether for memory pillow |
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Citations (9)
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2021
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