CN114213600A - Water-soluble polymer polyol and preparation method thereof - Google Patents

Water-soluble polymer polyol and preparation method thereof Download PDF

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CN114213600A
CN114213600A CN202111588428.9A CN202111588428A CN114213600A CN 114213600 A CN114213600 A CN 114213600A CN 202111588428 A CN202111588428 A CN 202111588428A CN 114213600 A CN114213600 A CN 114213600A
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polymer polyol
reaction
soluble polymer
water
styrene
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连江斌
苏国传
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Fujian Tianjiao Chemical Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F4/00Polymerisation catalysts
    • C08F4/28Oxygen or compounds releasing free oxygen
    • C08F4/32Organic compounds
    • C08F4/34Per-compounds with one peroxy-radical
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00Post-polymerisation treatments
    • C08F6/001Removal of residual monomers by physical means

Abstract

The invention discloses a water-soluble polymer polyol and a preparation method thereof, wherein the polymer polyol is prepared by the reaction of polyether polyol, styrene, acrylonitrile, hydrophilic group polyether graft, isopropanol and tert-amyl peroxy-2-ethyl hexanoate; the preparation method adopts a one-step method, and has the advantages of simple process, low cost and mild reaction; the hydrophilic group polyether graft has the characteristics of good water solubility and good dispersant property, the viscosity of the product is greatly reduced, the conversion rate of the product is increased from 98.5 percent to 99.0 percent, the amount of residual monomers is reduced, the preparation method is environment-friendly, the solid content of the product is high, the VOC is low, and the quality is more stable; the decomposed products of the tert-amyl peroxy-2-ethylhexanoate are all nontoxic oxygen-containing volatile gases with high purity, and compared with azodiisobutyronitrile, the product conversion rate is 5 per thousand higher and the VOC is low; meanwhile, a molecular removal technology and an oil-free vortex vacuum technology are introduced in the preparation process, the preparation method with the recovery amount of the residual monomers accounting for 5 per mill is environment-friendly, and the VOC is low; in significant contrast to current polymer polyol manufacturing processes.

Description

Water-soluble polymer polyol and preparation method thereof
Technical Field
The invention relates to the technical field of polymer chemistry and polyurethane materials, in particular to water-soluble polymer polyol and a preparation method thereof.
Background
Polymer polyols (POPs) based on Polyether Polyols (PPG) are prepared by reacting vinyl monomers, such as ethylene, acrylonitrile or styrene, in a polyol; POP is a main raw material for manufacturing the high-resilience polyurethane soft foam; the addition of polymer polyols to the foam-making formulation can improve the load-bearing properties of the foam; the soft polyurethane foam material prepared from POP is mainly divided into block-shaped soft foam and molded foam material, and has wide application; polyurethane block foams are used, among other things, in carpets, furniture and bedding, whereas polyurethane molded foams are used primarily in the automotive and aircraft industries.
Polymer polyols were first developed by United states carbide corporation (UCC), which established the first set of polymer polyol production facilities in 1964; at that time, acrylonitrile with the mass fraction of 5-20% is used as a vinyl monomer raw material, and polyether polyol with the average relative molecular mass of 3000 is used as a grafting parent body for industrial production; the product has yellow color, high viscosity and difficult storage, and is called first generation polymer polyol; in the middle of the 70 s, people introduce vinyl monomers such as styrene and the like and acrylonitrile for graft copolymerization to prepare white polymer polyol dispersion liquid, the product has low viscosity and excellent performance, the solid content is usually 20-30%, the mass ratio of the styrene to the acrylonitrile is 30/70-70/30, and the product is called second-generation polymer polyol or white polymer polyol; but the foam prepared by POP with the solid content within 30 percent cannot meet the requirements of higher load, rebound and low compression set; such as flexible foams with compressive hardness (ILD 25% deformation) greater than 100N, requiring POP solids above 40%; this POP is a third generation polymer polyol that has been developed in recent years, also known as a high solids polymer polyol.
The polyurethane foam plastic industry in China develops rapidly, and particularly, the polyurethane foam plastic has a great progress in the aspect of market development. The rapid development of domestic refrigeration and heat preservation, building energy conservation, solar industry, automobiles, furniture and other industries greatly draws the demand of polyurethane foam plastics, and the development center of gravity of polyurethane foam plastics is gradually shifted to China in the global range; among them, polyurethane foam has become one of the fastest-developing industries in the chemical industry in China.
Polyethers used in the synthesis of polyurethanes can be classified into three types — Polyether Polyols (PPG), polymer polyols (POP), and polytetramethylene glycols (PTMEG); among them, Polyether Polyol (PPG) and polymer polyol (POP) are important raw materials for the polyurethane industry, which account for about 90% of the polyether consumption; while polymer polyols are mainly used in the production of polyurethanes, the production and development of the polyurethane industry will determine its production and development.
As is well known, china produces 95% of the world's refrigerated containers, 60% of shoes and 70% of toys; the yields of building materials, spandex, textiles, synthetic leather and automobiles in China are all the first in the world; the urbanization process of China is accelerated, the investment of high-speed railways is increased, and the demand of environment-friendly synthetic wood is increased; the strong development of the industries brings huge market opportunities for the polyurethane industry in China and also provides wide market prospects for polyether products. However, most of polymer polyols in the current market have the problems of high viscosity, poor fluidity, poor water solubility, high VOC content and the like and yellow color of products; therefore, there is a need to develop a polymer polyol that meets the market demand and development trend, and has great significance for the development of polyether industry.
In view of the above, the present inventors have made extensive studies and studies to develop and design the present invention in view of the disadvantages and inconveniences caused by the above-mentioned incomplete improvement of the polymer polyol structure.
Disclosure of Invention
The invention aims to provide a water-soluble polymer polyol which has the advantages of good stability, low viscosity, high fluidity, good water solubility, low VOC and the like.
The invention also aims to provide a preparation method of the water-soluble polymer polyol, which not only has low viscosity and fine particles of the prepared polymer polyol, but also has good miscibility of the product with a small amount of water, and is beneficial to the later foaming operation; but also can increase the whiteness of the color of the product.
In order to achieve the above purpose, the solution of the invention is:
a water-soluble polymer polyol is prepared from the following components in parts by weight:
Figure BDA0003428816710000021
Figure BDA0003428816710000031
the solid content of the polymer polyol is 40-52%; the viscosity is 4000-7000mPa.s/25 ℃; styrene is less than or equal to 8 PPm.
Wherein the dosage of the hydrophilic group polyether graft is 10-20% of the total dosage of styrene and acrylonitrile.
A method for preparing a water-soluble polymer polyol, comprising the steps of:
the method comprises the following steps: mixing polyether polyol, styrene, acrylonitrile, hydrophilic group polyether graft, isopropanol and tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol.
After adopting the structure, the water-soluble polymer polyol and the preparation method thereof have the advantages of good stability, good dispersibility, good water solubility, low viscosity, low VOC (volatile organic compounds) and the like; has the following beneficial effects:
1. the polyether graft with hydrophilic groups is used as one of reaction monomers and reacts with styrene and acrylonitrile together, so that the synthesized polymer polyol dispersed phase particles have a dispersing agent function and a hydrophilic function, and the problem of poor fluidity in the downstream application process of the polymer polyol is solved;
2. the peroxide-2-ethyl hexanoic acid tert-amyl ester with higher purity is used as an initiator, all decomposers are nontoxic oxygen-containing volatile gases with high purity, and compared with azobisisobutyronitrile, the product conversion rate is 5 per thousand higher and the VOC is low;
3. meanwhile, a molecular removal technology and an oil-free vortex vacuum technology are introduced in the preparation process, the preparation method with the recovery amount of the residual monomers accounting for 5 per mill is environment-friendly, and the VOC is low;
4. the preparation method adopts a one-step method, and has simple process, low cost and mild reaction; the hydrophilic group polyether graft has the characteristics of good water solubility and good dispersant property, the viscosity of the product is greatly reduced, the conversion rate of the product is increased from 98.5 percent to 99.0 percent, the amount of residual monomers is reduced, the preparation method is environment-friendly, and the polymer polyol has high solid content, low VOC and more stable quality; in significant contrast to current polymer polyol manufacturing processes.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the embodiments of the present invention will be described in detail and completely with reference to the examples of the present invention, and it is apparent that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, provided in the examples, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention discloses a water-soluble polymer polyol which is prepared from the following components in parts by weight:
Figure BDA0003428816710000041
the solid content of the polymer polyol is 40-52%; the viscosity is 4000-7000mPa.s/25 ℃; styrene is less than or equal to 8 PPm.
The dosage of the hydrophilic group polyether graft is 10-20% of the total dosage of styrene and acrylonitrile.
The invention also discloses a preparation method of the water-soluble polymer polyol, which comprises the following steps:
the method comprises the following steps: mixing polyether polyol, styrene, acrylonitrile, hydrophilic group polyether graft, isopropanol and tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol.
The water-soluble polymer polyol and the preparation method thereof have the advantages of good stability, good dispersibility, good water solubility, low viscosity, low VOC (volatile organic compounds) and the like; has the following beneficial effects:
1. the polyether graft with hydrophilic groups is used as one of reaction monomers and reacts with styrene and acrylonitrile together, so that the synthesized polymer polyol dispersed phase particles have a dispersing agent function and a hydrophilic function, and the problem of poor fluidity in the downstream application process of the polymer polyol is solved;
2. the peroxide-2-ethyl hexanoic acid tert-amyl ester with higher purity is used as an initiator, all decomposers are nontoxic oxygen-containing volatile gases with high purity, and compared with azobisisobutyronitrile, the product conversion rate is 5 per thousand higher and the VOC is low;
3. meanwhile, a molecular removal technology and an oil-free vortex vacuum technology are introduced in the preparation process, the preparation method with the recovery amount of the residual monomers accounting for 5 per mill is environment-friendly, and the VOC is low;
4. the preparation method adopts a one-step method, and has simple process, low cost and mild reaction; the hydrophilic group polyether graft has the characteristics of good water solubility and good dispersant property, the viscosity of the product is greatly reduced, the conversion rate of the product is increased from 98.5 percent to 99.0 percent, the amount of residual monomers is reduced, the preparation method is environment-friendly, and the polymer polyol has high solid content, low VOC and more stable quality; in significant contrast to current polymer polyol manufacturing processes.
The main products of the invention, namely polyether glycol (PPG) and polymer polyol (POP), are important raw materials in the polyurethane industry, and the foamed plastic produced by polyurethane is widely applied to the fields of electronics, electric appliances, buildings, automobiles, packaging industry, furniture, shoe making, sealants, heat preservation, refrigeration and the like, belongs to the field of new material industry, and belongs to the encouragement industry (novel polyurethane series material matching raw materials) of China and Fujian provinces. Through the development of recent years, the polyurethane industry in China has a considerable scale from basic raw materials to products and mechanical equipment. With the development of the polyurethane industry, the market prospect of the polyether industry is further expanded.
After the invention is successfully researched and developed, the demand of the domestic market on high-end polyether products is fully met, so that the import quantity of similar products is reduced, a large amount of foreign exchanges are saved for the country, the problem of excess capacity of the domestic market is effectively relieved, the expected project amplification and pilot scale period can newly increase the yield value by 400 ten thousand yuan, the yield benefit is 64 ten thousand yuan, the annual profit is 40 ten thousand yuan, and the invention has good social benefit and economic benefit.
The beneficial effects are further illustrated by the following sets of examples:
example 1
The method comprises the following steps: mixing 25 parts of polyether polyol, 35 parts of styrene, 30 parts of acrylonitrile, 8.4 parts of hydrophilic group polyether graft, 0.8 part of isopropanol and 0.8 part of tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 64.30%; the viscosity is 5800mPa.s/25 ℃; styrene 6 ppm.
Example 2
The method comprises the following steps: mixing 40 parts of polyether polyol, 30 parts of styrene, 22 parts of acrylonitrile, 6.4 parts of hydrophilic group polyether graft, 0.8 part of isopropanol and 0.8 part of tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 51.40%; the viscosity is 5100mPa.s/25 ℃; styrene 5 ppm.
Example 3
The method comprises the following steps: mixing 55 parts of polyether polyol, 26 parts of styrene, 13 parts of acrylonitrile, 4.4 parts of hydrophilic group polyether graft, 0.8 part of isopropanol and 0.8 part of tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 38.90%; the viscosity is 4100mPa.s/25 ℃; styrene 3 ppm.
Example 4
The method comprises the following steps: mixing 40 parts of polyether polyol, 30 parts of styrene, 14 parts of acrylonitrile, 5 parts of hydrophilic group polyether graft, 0.5 part of isopropanol and 0.5 part of tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 48.6%; the viscosity is 5100mPa.s/25 ℃; styrene 5 ppm.
Example 5
The method comprises the following steps: mixing 40 parts of polyether polyol, 30 parts of styrene, 14 parts of acrylonitrile, 10 parts of hydrophilic group polyether graft, 0.5 part of isopropanol and 0.5 part of tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 46.2%; the viscosity is 4300mPa.s/25 ℃; styrene 3 ppm.
Example 6
The method comprises the following steps: mixing 35 parts of polyether polyol, 30 parts of styrene, 14 parts of acrylonitrile, 5 parts of hydrophilic group polyether graft, 0.5 part of isopropanol and 0.5 part of tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 51.2%; the viscosity is 6200mPa.s/25 ℃; styrene 7 ppm.
Example 7
The method comprises the following steps: mixing 25 parts of polyether polyol, 25 parts of styrene, 10 parts of acrylonitrile, 3 parts of hydrophilic group polyether graft, 0.2 part of isopropanol and 0.1 part of peroxide-2-ethyl hexanoate under normal temperature and pressure to prepare reaction liquid;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 55.30%; the viscosity is 5800mPa.s/25 ℃; styrene 6 ppm.
Example 8
The method comprises the following steps: mixing 30 parts of polyether polyol, 28 parts of styrene, 15 parts of acrylonitrile, 4 parts of hydrophilic group polyether graft, 0.3 part of isopropanol and 0.3 part of tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 55.40%; the viscosity is 6000mPa.s/25 ℃; styrene 5 ppm.
Example 9
The method comprises the following steps: mixing 35 parts of polyether polyol, 30 parts of styrene, 20 parts of acrylonitrile, 6 parts of hydrophilic group polyether graft, 0.5 part of isopropanol and 0.5 part of tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 54.30%; the viscosity is 5600mPa.s/25 ℃; styrene 3 ppm.
Example 10
The method comprises the following steps: mixing 40 parts of polyether polyol, 32 parts of styrene, 25 parts of acrylonitrile, 8 parts of hydrophilic group polyether graft, 0.8 part of isopropanol and 0.8 part of tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 53.50%; the viscosity is 5200mPa.s/25 ℃; styrene 7 ppm.
Example 11
The method comprises the following steps: mixing 55 parts of polyether polyol, 35 parts of styrene, 30 parts of acrylonitrile, 10 parts of hydrophilic group polyether graft, 1 part of isopropanol and 1 part of tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol. The polymer polyol solids content was 49.20%; the viscosity is 4800mPa.s/25 ℃; styrene 5 ppm.
TABLE 1 test data for water-soluble polymer polyols made in the examples
Figure BDA0003428816710000111
As can be seen from the above table, the water-soluble polymer polyol of the invention has a solid content of 35-70%, a viscosity of 4000-7000mPa.s/25 ℃, a styrene content of less than or equal to 8mg/kg, a pH value of 6-9, and a milky white or slightly yellowish white viscous liquid appearance; has the characteristics of better stability, low viscosity and low VOC.
The above embodiments are not intended to limit the form and style of the present invention, and any suitable changes or modifications made by those skilled in the art should be considered as not departing from the scope of the present invention.

Claims (4)

1. The water-soluble polymer polyol is characterized by being prepared from the following components in parts by weight:
Figure FDA0003428816700000011
2. the water-soluble polymer polyol of claim 1, wherein: the solid content of the polymer polyol is 40-52%; the viscosity is 4000-7000mPa.s/25 ℃; styrene is less than or equal to 8 PPm.
3. The water-soluble polymer polyol of claim 1, wherein: wherein the dosage of the hydrophilic group polyether graft is 10-20% of the total dosage of styrene and acrylonitrile.
4. The method for producing a water-soluble polymer polyol according to any one of claims 1 to 3, comprising the steps of:
the method comprises the following steps: mixing polyether polyol, styrene, acrylonitrile, hydrophilic group polyether graft, isopropanol and tert-amyl peroxy-2-ethylhexanoate at normal temperature and pressure to prepare a reaction solution;
step two: continuously injecting the reaction liquid into a reaction kettle for polymerization reaction, controlling the reaction temperature to be 125-135 ℃, controlling the reaction pressure to be 0.3-0.5 MPa, and controlling the residence time of the reaction materials to be 2 hours to prepare polymer polyol;
step three: and (3) subjecting the prepared polymer polyol to molecular removal and oil-free vortex vacuum treatment, performing vacuum demonomerization for 3-4 hours at the temperature of 150-170 ℃ and under the pressure of-0.08 to-0.1 MPa, removing and recovering micromolecular substances, and finally preparing the required water-soluble polymer polyol.
CN202111588428.9A 2021-12-23 2021-12-23 Water-soluble polymer polyol and preparation method thereof Pending CN114213600A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115043990A (en) * 2022-07-26 2022-09-13 上海华谊(集团)公司 Production process of low-VOC polymer polyol

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115043990A (en) * 2022-07-26 2022-09-13 上海华谊(集团)公司 Production process of low-VOC polymer polyol

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