阅读说明：本技术 一种弹性阻燃聚醚多元醇及其制备方法 (Elastic flame-retardant polyether polyol and preparation method thereof ) 是由 陆华欧 黄豪 庄焕明 于 2021-01-08 设计创作，主要内容包括：本发明公开了一种弹性阻燃聚醚多元醇及其制备方法,属于聚醚多元醇技术领域,由下列成分按照重量份配制而成,配方为：三聚氰胺10-16份、慢回弹聚醚多元醇1-5份、多聚甲醛1-5份、环氧丙烷75-85份和三乙胺0.1-0.5份。先将三聚氰胺、多聚甲醛混合均匀；再将混合液升至75～85℃在常压环境下反应1～2小时,制得前驱体；之后加入慢回弹聚醚多元醇、环氧丙烷、三乙胺混合均匀,升至90-110℃,常压下持续反应4-8小时；最后在高真空状态下通入惰性气体,将水分、环氧丙烷等小分子脱除,制得弹性阻燃聚醚多元醇。本发明的有益效果是本发明得到的聚醚物多元醇,具有无卤素、阻燃效率高、挥发性小、分解温度高、低毒、不产生腐蚀性气体,废物不会造成二次污染等特性并且能够提高产率。(The invention discloses an elastic flame-retardant polyether polyol and a preparation method thereof, belonging to the technical field of polyether polyols, and the elastic flame-retardant polyether polyol is prepared from the following components in parts by weight: 10-16 parts of melamine, 1-5 parts of slow rebound polyether polyol, 1-5 parts of paraformaldehyde, 75-85 parts of propylene oxide and 0.1-0.5 part of triethylamine. Firstly, uniformly mixing melamine and paraformaldehyde; raising the temperature of the mixed solution to 75-85 ℃ and reacting for 1-2 hours under normal pressure environment to prepare a precursor; then adding slow-rebound polyether polyol, propylene oxide and triethylamine, uniformly mixing, heating to 90-110 ℃, and continuously reacting for 4-8 hours under normal pressure; and finally, introducing inert gas in a high vacuum state to remove water, propylene oxide and other micromolecules to prepare the elastic flame-retardant polyether polyol. The polyether polyol obtained by the invention has the characteristics of no halogen, high flame retardant efficiency, low volatility, high decomposition temperature, low toxicity, no generation of corrosive gas, no secondary pollution caused by waste and the like, and can improve the yield.)

1. The elastic flame-retardant polyether polyol is characterized by being prepared from the following components in parts by weight:

10-16 parts of melamine

1-5 parts of slow rebound polyether polyol

1-5 parts of paraformaldehyde

75-85 parts of propylene oxide

0.1-0.5 part of triethylamine.

2. An elastomeric flame retardant polyether polyol according to claim 1, wherein the slow rebound polyether polyol is a slow rebound polyether polyol having a hydroxyl value of 300 ± 10mgKOH/g or 240 ± 10 mgKOH/g.

3. The elastic flame-retardant polyether polyol according to claim 2, wherein the water content is 0.15% or less, the viscosity is 1500mpa.s/25 ℃ or more, the nitrogen content is 1% or more, and the oxygen index of the synthesized polyurethane product is 25% or more.

4. The elastic flame-retardant polyether polyol as claimed in claim 3, which is prepared from the following components in parts by weight:

15.3 portions of melamine

2 parts of slow rebound polyether polyol

1.4 parts of paraformaldehyde

81 parts of propylene oxide

And 0.3 part of triethylamine.

5. The flexible, flame-retardant polyether polyol according to claim 4, wherein the water content is 0.14%, the viscosity is 6312mPa.s/25 ℃, the nitrogen content is 9%, and the oxygen index of the resultant polyurethane product is 25.5%.

6. A process for the preparation of an elastomeric flame retardant polyether polyol according to any of claims 1-5, characterized in that it comprises the steps of:

step one, melamine and paraformaldehyde are uniformly mixed;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding the product of the step two into slow rebound polyether polyol, propylene oxide and triethylamine, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

7. The method for preparing an elastic flame-retardant polyether polyol according to claim 6, wherein: in the first step, the pH value of the mixed solution of melamine and paraformaldehyde is between 8 and 9.

8. The method of claim 7, wherein the method comprises the steps of: and in the first step, the pH value of the mixed solution is adjusted by adopting a NaOH solution.

9. The method of claim 8, wherein the method comprises the steps of: and in the second step, the temperature of the mixed solution is increased to 80-82 ℃.

10. The method of claim 9, wherein the method comprises the steps of: and step three, heating the mixed solution to 100-102 ℃.

Technical Field

The invention relates to the technical field of polyether polyol, and particularly relates to elastic flame-retardant polyether polyol and a preparation method thereof.

Background

Zhang Tianlin et al prepared bromine-containing flame-retardant polyether polyol by using pentabromophenyl glycidyl ether, propylene oxide and ethylene oxide as raw materials. When the mass fraction of the flame-retardant polyether polyol added into the formula is 23%, the oxygen index of the product can reach 28.5%. The polyurethane material synthesized by the halogen flame-retardant polyol can emit toxic gas during combustion to cause secondary damage, and the use of halogen flame-retardant is gradually restricted along with the improvement of the environmental protection requirement.

Li Yan et al uses trihydroxy methyl oxyphosphor and epoxypropane as main raw materials to prepare a phosphorus-containing polyether polyol, and then uses the phosphorus-containing polyether polyol as a raw material to prepare a polyurethane material, compared with a polyurethane material prepared by using common polyether polyol, the limiting oxygen index can reach 25.6%. Polyurethane materials synthesized from phosphorus-based flame-retardant polyols release a large amount of smoke during combustion, and phosphorus-containing substances have high volatility and poor thermal stability.

Compared with the polyurethane material prepared by common polyether polyol, the polyurethane material prepared by the nitrogen-containing flame-retardant polyether polyol is superior to the polyurethane material prepared by the common polyether in both limit oxygen index and smoke density, and the limit oxygen index can reach 24.3%. Polyurethane materials synthesized from nitrogen-based flame retardant polyols decompose to release non-combustible gases such as ammonia, nitrogen oxides, water vapor and the like during combustion, thereby reducing the concentration of oxygen in the air. Meanwhile, a large amount of heat is absorbed, the temperature of the surface of the polymer is greatly reduced, and the smoke generation amount is small.

The flame-retardant polyether polyol is developed by Jiangyin Youbang chemical company Limited, and the polyether polyol without halogen, phosphorus, antimony and other elements is synthesized by grafting a nitrogen heterocyclic structure unit in high-activity polyether. The product is milky viscous liquid, the average diameter of particles is 0.2 mu m, and the viscosity is 2000m Pa & s; the oxygen index of the foam product prepared by the method can reach 26%, the smell is small during combustion, and the smoke density is less than or equal to 60%.

In the current research progress, the nitrogen-based flame-retardant polyether polyol has absolute advantages in the aspect of environmental protection and accords with the current social development trend. However, the existing nitrogen-series flame-retardant polyether polyol still has the defects of flame retardance, safety performance, volatility, production cost and product structure stability.

Disclosure of Invention

Aiming at the problems of flame retardance, safety performance, production cost and the like of nitrogen-series flame-retardant polyether polyol in the prior art, the invention provides elastic flame-retardant polyether polyol which is prepared from the following components in parts by weight:

10-16 parts of melamine

1-5 parts of slow rebound polyether polyol

1-5 parts of paraformaldehyde

75-85 parts of propylene oxide

0.1-0.5 part of triethylamine.

Preferably, the slow rebound polyether polyol is a slow rebound polyether polyol having a hydroxyl value of 300 + -10 mgKOH/g or 240 + -10 mgKOH/g.

Preferably, the water content is less than or equal to 0.15%, the viscosity is greater than or equal to 1500mPa.s/25 ℃, the nitrogen content is greater than or equal to 1%, and the oxygen index of the synthesized polyurethane product is more than 25%.

Preferably, the composition is prepared from the following components in parts by weight:

15.3 portions of melamine

2 parts of slow rebound polyether polyol

1.4 parts of paraformaldehyde

81 parts of propylene oxide

And 0.3 part of triethylamine.

Preferably, the water content is 0.14%, the viscosity is 6312mPa.s/25 ℃, the nitrogen content is 9%, and the oxygen index of the synthesized polyurethane product is 25.5%.

The invention also relates to a preparation method of the elastic flame-retardant polyether polyol, which comprises the following steps:

step one, melamine and paraformaldehyde are uniformly mixed;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding the product of the step two into slow rebound polyether polyol, propylene oxide and triethylamine, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Preferably, the pH value of the mixed solution of melamine and paraformaldehyde in the first step is between 8 and 9.

Preferably, in the first step, a NaOH solution is used to adjust the pH value of the mixed solution.

Preferably, the temperature of the mixed solution in the second step is increased to 80-82 ℃.

Preferably, the temperature of the mixed solution in the third step is increased to 100-102 ℃.

By utilizing the principle of anion ring-opening polymerization reaction, melamine with flame retardant property is introduced into the molecular structure of the slow rebound polyether polyol, and the amine group of the melamine is subjected to dehydration condensation with formaldehyde to methylate the terminal group hydroxyl group of the melamine to be used as a precursor of the slow rebound polyether polyol addition reaction. The prepared melamine-containing precursor, slow-rebound polyether polyol and propylene oxide are subjected to ring-opening addition catalyzed by triethylamine to prepare the elastic flame-retardant polyether polyol.

Has the advantages that:

the technical scheme of the invention has the following beneficial effects:

(1) by utilizing the principle of anion ring-opening polymerization reaction, melamine with flame retardant property is introduced into the molecular structure of the slow rebound polyether polyol, and the amine group of the melamine is subjected to dehydration condensation with formaldehyde to methylate the terminal group hydroxyl group of the melamine to be used as a precursor of the slow rebound polyether polyol addition reaction. The prepared melamine-containing precursor, slow-rebound polyether polyol and propylene oxide are subjected to ring-opening addition catalyzed by triethylamine to prepare the elastic flame-retardant polyether polyol.

(2) The polyether polyol obtained by the reaction of the epoxypropane and the precursor has the characteristics of no halogen, high flame-retardant efficiency, small volatility, high decomposition temperature, low toxicity, no generation of corrosive gas, no secondary pollution caused by waste and the like. The polyamine is a coinitiator, which can effectively adjust the hydroxyl value and viscosity of the product and simultaneously initiate the reaction of the poly-methylol melamine and the propylene oxide, thereby improving the yield.

Detailed Description

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 embodiment provides elastic flame-retardant polyether polyol which is prepared from the following components in parts by weight:

10-16 parts of melamine

1-5 parts of slow rebound polyether polyol

1-5 parts of paraformaldehyde

75-85 parts of propylene oxide

0.1-0.5 part of triethylamine.

As a preferred embodiment, the slow rebound polyether polyol is a slow rebound polyether polyol having a hydroxyl value of 300. + -. 10mgKOH/g or 240. + -. 10 mgKOH/g.

In a preferred embodiment, the water content is less than or equal to 0.15%, the viscosity is greater than or equal to 1500mPa.s/25 ℃, the nitrogen content is greater than or equal to 1%, and the oxygen index of the synthesized polyurethane product is more than 25%.

The preparation is prepared from the following components in parts by weight:

15.3 portions of melamine

2 parts of slow rebound polyether polyol

1.4 parts of paraformaldehyde

81 parts of propylene oxide

And 0.3 part of triethylamine.

In a preferred embodiment, the water content is 0.14%, the viscosity is 6312mPa.s/25 ℃, the nitrogen content is 9%, and the oxygen index of the synthesized polyurethane product is 25.5%.

The embodiment also relates to a preparation method of the elastic flame-retardant polyether polyol, which comprises the following steps:

step one, melamine and paraformaldehyde are uniformly mixed;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding the product of the step two into slow rebound polyether polyol, propylene oxide and triethylamine, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

In a preferred embodiment, the pH of the mixture of melamine and paraformaldehyde in step one is between 8 and 9.

In a preferred embodiment, the pH of the mixture is adjusted in step one with NaOH solution.

In a preferred embodiment, the temperature of the mixed solution in the second step is raised to 80-82 ℃.

In a preferred embodiment, the temperature of the mixed solution in the third step is raised to 100 to 102 ℃.

By utilizing the principle of anion ring-opening polymerization reaction, melamine with flame retardant property is introduced into the molecular structure of the slow rebound polyether polyol, and the amine group of the melamine is subjected to dehydration condensation with formaldehyde to methylate the terminal group hydroxyl group of the melamine to be used as a precursor of the slow rebound polyether polyol addition reaction. The prepared melamine-containing precursor, slow-rebound polyether polyol and propylene oxide are subjected to ring-opening addition catalyzed by triethylamine to prepare the elastic flame-retardant polyether polyol.

The elastic flame-retardant polyether polyol obtained by the technical scheme of the embodiment is further illustrated by the following groups of examples and comparative examples.

Example one

The preparation method of the elastic flame-retardant polyether polyol in the embodiment comprises the following steps:

step one, evenly mixing 10 parts of melamine and 5 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 1 part of slow rebound polyether polyol, 83.9 parts of propylene oxide and 0.1 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 300 +/-10 mgKOH/g.

Example two

The preparation method of the elastic flame-retardant polyether polyol in the embodiment comprises the following steps:

the invention also relates to a preparation method of the elastic flame-retardant polyether polyol, which comprises the following steps:

step one, uniformly mixing 16 parts of melamine and 3.5 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 5 parts of slow rebound polyether polyol, 75 parts of propylene oxide and 0.5 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 300 +/-10 mgKOH/g.

EXAMPLE III

The preparation method of the elastic flame-retardant polyether polyol in the embodiment comprises the following steps:

step one, evenly mixing 12 parts of melamine and 1 part of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 1.7 parts of slow rebound polyether polyol, 85 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Example four

The preparation method of the elastic flame-retardant polyether polyol in the embodiment comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example 1

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde uniformly;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example No. two

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, 8 parts of melamine and 1.4 parts of paraformaldehyde are uniformly mixed;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example No. three

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, evenly mixing 18 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example No. four

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 0.5 part of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example five

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 7 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example six

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 0.5 part of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example seven

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 7 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example eight

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 73 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example No. nine

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 88 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example ten

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 320 mgKOH/g.

Comparative example eleven

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is slow rebound polyether polyol comparative example twelve with hydroxyl value of 280mgKOH/g

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 220 mgKOH/g.

Comparative example thirteen

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 260 mgKOH/g.

Comparative example fourteen

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 90 ℃ to perform reaction under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 90-110 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

Comparative example fifteen

The preparation method of the elastic flame-retardant polyether polyol in the comparative example comprises the following steps:

step one, uniformly mixing 15.3 parts of melamine and 1.4 parts of paraformaldehyde;

step two, heating the mixed solution obtained in the step one to 75-85 ℃, and reacting under a normal pressure environment for 1-2 hours to obtain a precursor;

step three, adding 2 parts of slow rebound polyether polyol, 81 parts of propylene oxide and 0.3 part of triethylamine into the product obtained in the step two, uniformly mixing, heating to 80 ℃, maintaining the pressure at normal pressure, and continuously reacting for 4-8 hours;

and step four, introducing inert gas in a high vacuum state, and removing small molecules such as moisture, propylene oxide and the like to prepare the required elastic flame-retardant polyether polyol.

Wherein the slow rebound polyether polyol is the slow rebound polyether polyol with the hydroxyl value of 240 +/-10 mgKOH/g.

The elastic flame-retardant polyether polyol prepared in the four groups of examples and the fifteen groups of comparative examples is tested, and the specific data is as follows:

TABLE 1 test data for elastomeric flame retardant polyether polyols obtained from the examples and comparative examples

From the data of four groups of examples and fifteen groups of comparative examples in the table, we can find that the elastic flame-retardant polyether polyol and the preparation method thereof can keep higher nitrogen content and oxygen index while keeping lower water content and better viscosity.

The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.