CN110628009A

CN110628009A - Polyether polyol for self-opening low-temperature soft slow-rebound mattress foam and preparation method thereof, and slow-rebound foam and preparation method thereof

Info

Publication number: CN110628009A
Application number: CN201910908751.6A
Authority: CN
Inventors: 王文涛; 孙兆任; 李剑锋; 公维英; 周玉波
Original assignee: Shandong Inov New Material Co Ltd
Current assignee: Shandong Inov New Material Co Ltd
Priority date: 2019-09-25
Filing date: 2019-09-25
Publication date: 2019-12-31

Abstract

The invention belongs to the technical field of chemical preparation, and particularly relates to polyether polyol for self-opening low-temperature soft slow-rebound mattress foam, a preparation method of the polyether polyol, slow-rebound foam and a preparation method of the slow-rebound foam. The polyether polyol is prepared by copolymerization of a special initiator serving as a raw material and propylene oxide and ethylene oxide. The slow rebound foam is prepared from a component A and a component B, wherein the component A is polyether polyol 1, the polyether polyol of the invention, polymer polyol, a catalyst, a foam stabilizer and a foaming agent, and the component B is a mixture of T80 and DG 5412; a, B components are mixed evenly and poured into a mould for curing to obtain the slow-rebound foam. The slow rebound foam prepared by the polyether polyol prepared by the invention is self-opened, the opening rate can reach 75.6 percent, the foam is soft at low temperature and does not harden, the hand feeling is comfortable, and the problems of poor opening performance and low-temperature hardening of the current slow rebound foam can be effectively solved.

Description

Polyether polyol for self-opening low-temperature soft slow-rebound mattress foam and preparation method thereof, and slow-rebound foam and preparation method thereof

Technical Field

The invention belongs to the technical field of chemical preparation, and particularly relates to polyether polyol for self-opening low-temperature soft slow-rebound mattress foam, a preparation method of the polyether polyol, slow-rebound foam and a preparation method of the slow-rebound foam.

Background

The slow rebound polyurethane foam is a foam material with viscoelasticity, when the foam is deformed under the action of external force, the strain lags behind the change of stress, so that when the foam is subjected to the external force, the foam does not recover immediately, but slowly recovers to the original shape after 3-15 seconds, and the slow rebound polyurethane foam has the memory property, namely the memory foam. Therefore, the slow rebound foam is widely applied to various cushion materials, such as pillows, mattresses, waist pillows, neck protectors, mattresses and the like, and compared with the traditional cushion material, the slow rebound foam can reduce the extrusion sense to the human body, is beneficial to blood circulation and has higher comfort.

In a slow rebound formula system, generally, the pore wall formed by polyether polyol and isocyanate is difficult to break by gas, the phenomena of serious closed pore and obvious shrinkage often occur, and good openness does not exist, which means that the dimensional stability is poor and the comfort is greatly reduced for foam, thus bringing great inconvenience to industrial production and product application. In addition, in the field of slow rebound sound insulation application, the added pore opening agent can bring rough surface of a product and influence the service life of the material, so that the development of polyether polyol with the pore opening property has great application value. In the application of the slow rebound material, another main problem which troubles the product is the hardening phenomenon of the product in winter, the product loses the slow rebound effect and the use value is lost.

Disclosure of Invention

The technical problem to be solved by the invention is as follows: the polyether polyol for the self-opening low-temperature soft slow-rebound mattress foam overcomes the defects of the prior art, is used as the main polyether of the slow-rebound formula, does not need to be added with a cell opening agent, and has good opening effect of the prepared foam, softness, comfort, no hardness and good performance under the low-temperature condition; the invention also provides a preparation method of the compound, which is simple and easy to operate.

The invention also provides the slow rebound foam prepared by the polyether polyol for the self-opening low-temperature soft slow rebound mattress foam, a cell opening agent is not required to be added, the cell opening effect is good, the slow rebound foam is soft and comfortable under the low-temperature condition, does not harden, and has good performances.

The polyether glycol for the self-opening low-temperature soft slow-rebound mattress foam is prepared by copolymerizing an initiator A, an initiator B and alkylene oxide under the action of a catalyst, wherein,

the initiator A is one of n-amyl alcohol, n-hexyl alcohol, n-heptyl alcohol or n-octyl alcohol;

the initiator B is one of propylene glycol, glycerol or pentaerythritol;

the molar ratio of the initiator A to the initiator B is that of the initiator A: starter B ═ 1: 4-2: 3;

the alkylene oxide is propylene oxide and ethylene oxide;

the hydroxyl value of the polyether polyol is 22.0-27.0mgKOH/g, the epoxy propane accounts for 23-34 wt% of the molecular chain, and the epoxy ethane accounts for 65-75 wt%.

Wherein:

the catalyst is one of a phosphazene catalyst, a double metal cyanide complex catalyst or KOH.

The preparation method of the polyether polyol for the self-opening low-temperature soft slow-rebound mattress foam comprises the following steps:

1) adding the initiator A, the initiator B and the catalyst in the formula amount into a high-pressure reaction kettle, replacing with nitrogen until the oxygen content is less than or equal to 50ppm, heating to 80-100 ℃, keeping the vacuum degree at-0.095 MPa, and vacuumizing and dehydrating for 0.5-2 h;

2) continuously adding propylene oxide accounting for 5 percent of the total mass of the polyether polyol to react, wherein the temperature is 78-82 ℃, stopping feeding when the designed amount is reached, and heating to 112 ℃ along with 108 ℃;

3) continuously adding 18-29% of propylene oxide and 57-67% of ethylene oxide based on the total mass of polyether polyol for polymerization, stopping feeding when the design amount is reached, and continuing aging reaction for 1-2 h;

4) continuously adding ethylene oxide accounting for 8 percent of the total mass of polyether polyol for polymerization, stopping feeding when the design amount is reached, aging for 1-2h, and vacuumizing for 0.5-1 h;

5) and cooling to 80-90 ℃, adding phosphoric acid, water and an adsorbent for post-treatment, and performing suction filtration to obtain the target polyether polyol.

The slow rebound foam prepared by adopting the polyether polyol for the self-opening low-temperature soft slow rebound mattress foam consists of A, B components,

the component A is prepared from the following raw materials in parts by weight:

130-40 parts of polyether polyol;

235-40 parts of polyether polyol;

20-35 parts of polymer polyol;

0.45-0.65 part of catalyst;

1.0-2.0 parts of foam stabilizer;

1-3 parts of a foaming agent;

the component B is a mixture of T80 and DG5412, and the isocyanate index is 0.9%;

wherein:

polyether polyol 1 is INOVOL F5631;

polyether polyol 2 is the polyether polyol for self-opening, low temperature soft slow rebound mattress foam of claim 1 or 2.

The polymer polyol is POP 2045.

The catalyst is a mixture of A33 and T9.

The foam stabilizer is an organic silicon foam stabilizer L580.

The foaming agent is water.

The mass ratio of the T80 to the DG5412 is 7: 3-8: 2.

the preparation method of the slow rebound foam comprises the following steps:

1) uniformly stirring polyether polyol 1, polyether polyol 2, polymer polyol, a catalyst, a foam stabilizer and a foaming agent according to the formula ratio at room temperature;

2) adding the isocyanate component B according to the formula amount, stirring the component A and the component B for 4-5s, pouring into a mold, and curing at normal temperature for 24-48 hours to obtain the target product.

The invention has the following beneficial effects:

(1) the polyether polyol prepared by the invention adopts a unique composite initiator design structure, and the molecular structure of the polyether polyol is designed by controlling the proportion of alkylene oxide, so that the prepared slow rebound foam has the characteristics of low temperature softness and no hardening.

(2) The polyether polyol prepared by the invention can be used as main polyether of a slow rebound formula, a pore-forming agent is not required to be added, the pore-forming effect is good, the cost is relatively low, the formula design can be simplified, and the use is convenient.

(3) The slow-rebound foam prepared by the invention has the advantages of simple process flow, excellent foam mechanical property, temperature and humidity sensitivity index of less than 1.1 under low temperature condition and comfortable hand feeling.

(4) The preparation method is simple and easy to operate.

Detailed Description

The present invention is further illustrated by, but is not limited to, the following examples.

All the starting materials used in the examples are commercially available, except where otherwise indicated.

Example 1

The polyether polyol for the self-opening low-temperature soft slow-rebound mattress foam and the preparation method thereof comprise the following steps:

1) 306.5g of n-amyl alcohol, 736g of glycerol and 171.8g of catalyst KOH are added into a high-pressure reaction kettle, nitrogen is replaced until the oxygen content is less than or equal to 50ppm, the temperature is raised to 80 ℃, and the vacuum degree is maintained at-0.095 MPa, and the vacuum pumping dehydration is carried out for 0.5 h;

2) gradually and continuously adding 3436g of Propylene Oxide (PO) for reaction, controlling the polymerization reaction temperature to be 80 +/-2 ℃, stopping feeding when the PO design amount is reached, and starting to heat to 110 +/-2 ℃;

3) continuously adding 19585g of Propylene Oxide (PO) and 39170.4g of Ethylene Oxide (EO) for polymerization, stopping feeding when the design amount is reached, and continuing the aging reaction for 2 hours;

4) 5497.6g of Ethylene Oxide (EO) is continuously added for polymerization, the feeding is stopped when the design amount is reached, the aging is carried out for 1h, and the vacuumizing is carried out for 0.5 h;

5) and cooling to 80 ℃, adding 406.3g of phosphoric acid, 2405.5g of water and 137g of adsorbent for post-treatment, and performing suction filtration to obtain the target polyether polyol 1 (hydroxyl value is 25.2mg KOH/g).

Example 2

1) 520.9g of n-octanol, 816.9g of pentaerythritol and 172g of catalyst KOH are added into a high-pressure reaction kettle, nitrogen is replaced until the oxygen content is less than or equal to 50ppm, the temperature is raised to 100 ℃, and the vacuum degree is maintained at-0.095 MPa, and the vacuum pumping and the dehydration are carried out for 2 hours;

2) 3436g of Propylene Oxide (PO) was continuously added to carry out the reaction, the polymerization temperature was controlled to 80. + -. 2 ℃ and when the designed amount of PO was reached, the addition was stopped and the temperature was raised to 110. + -. 2 ℃.

3) Continuously adding 12438g of Propylene Oxide (PO) and 46042.4g of Ethylene Oxide (EO) for polymerization, stopping feeding when the design amount is reached, and continuing the aging reaction for 1.5 h;

4) 5497.6g of Ethylene Oxide (EO) is continuously added for polymerization, the feeding is stopped when the design amount is reached, the aging is carried out for 2h, and the vacuumizing is carried out for 1 h;

5) and cooling to 85 ℃, adding 405.9g of phosphoric acid, 2749.2g of water and 69g of adsorbent for post-treatment, and performing suction filtration to obtain the target polyether polyol 2 (hydroxyl value is 22.9 mgKOH/g).

Example 3

1) adding 500.9g of n-hexanol, 1021.1g of pentaerythritol and 206.2g of catalyst KOH into a high-pressure reaction kettle, replacing with nitrogen until the oxygen content is less than or equal to 50ppm, heating to 90 ℃, keeping the vacuum degree at-0.095 MPa, and performing vacuum-pumping dehydration for 1 h;

3) Continuously adding 15874g of Propylene Oxide (PO) and 42606.4g of Ethylene Oxide (EO) for polymerization, stopping feeding when the design amount is reached, and continuing the aging reaction for 1 hour;

4) 5497.6g of Ethylene Oxide (EO) is continuously added for polymerization, the feeding is stopped when the design amount is reached, the aging is carried out for 1.5h, and the vacuumizing is carried out for 0.7 h;

5) the temperature is reduced to 90 ℃, 488.7g of phosphoric acid, 2062g of water and 34g of adsorbent are added for post-treatment, and the target polyether polyol 3 (hydroxyl value is 26.5mgKOH/g) is obtained by suction filtration.

The following are the applications and performance tests of the self-open low temperature soft slow rebound mattress foam synthesized by the present invention.

Recovery time, s: GB/T24451-;

temperature sensitivity coefficient: GB/T24451-;

tensile strength, kPa: GB/T6344-2008;

tear strength, N/m: GB/T6344-2008;

density, kg/m³：GB/T6343-1995。

The formulations and performance test results for the self-open, low temperature, soft, slow rebound mattress foams prepared using the polyether polyols prepared in the examples are shown in tables 1 and 2.

The preparation method of the slow rebound foam comprises the following steps:

1) the INOVOL F5631, the slow rebound polyether, POP2045, the catalyst, the foam stabilizer and the water in the formula amount are stirred uniformly at room temperature of 25 ℃;

2) adding the isocyanate component B according to the formula amount, stirring the component A and the component B for 5s, pouring into a mold, and curing at normal temperature for 24 hours to obtain the target product.

Wherein:

example 4 and example 7 the polyether polyol prepared in example 1 was used;

examples 5 and 8 the polyether polyol prepared in example 2 was used;

example 6 and example 9 the polyether polyol prepared in example 2 was used.

The mass ratio of the catalyst A33 to the catalyst T9 is 1: 1.

the inocol F1070A type polyether polyol used in comparative examples 1 and 2 is a small molecular weight polyether polyol for slow rebound foam, which is used in place of the slow rebound polyether of the present invention. Comparative examples 1 and 2 were prepared in the same manner as in examples 4 to 9.

TABLE 1

	Example 4	Example 5	Example 6	Comparative example 1
					INOVOL F5631	30	30	30	30
The slow rebound polyether of the invention	35	35	35	0
					POP 2045	35	35	35	35
INOVOL F1070A	0	0	0	35
					L580	1.0	1.0	1.0	1.0
Water (W)	1	1	1	1
					A33/T9	0.65	0.65	0.65	0.65
T80	12.8	12.9	13.1	24.3
					DG5412	3.2	3.2	3.3	6.1
Isocyanate index	0.9	0.9	0.9	0.9
					Open cell content%	62.9％	66.8％	72.1％	52.6％
Density of foam	87.9	87.5	87.4	87.6
					Recovery time/s	8	9	9	5
Temperature coefficient of sensitivity	1.05	1.01	1.06	1.35
					Tensile Strength/kPa	82	88	84	70
Tear Strength/N/m	286	290	282	235

TABLE 2

	Example 7	Example 8	Example 9	Comparative example 2
					INOVOL F5631	40	40	40	40
The slow rebound polyether of the invention	40	40	40	0
					POP 2045	20	20	20	20
INOVOL F1070A	0	0	0	40
					L580	2.0	2.0	2.0	2.0
Water (W)	3	3	3	3
					A33/T9	0.45	0.45	0.45	0.45
T80	27	27.1	27.3	36.5
					DG5412	11.6	11.6	11.7	15.7
Isocyanate index	0.9	0.9	0.9	0.9
					Open cell content%	67.5％	70.2％	75.6％	50.4％
Density of foam	54.2	54.4	53.9	54.0
					Recovery time/s	9	10	10	5
Temperature coefficient of sensitivity	0.99	0.94	0.96	1.27
					Tensile Strength/kPa	75	80	78	65
Tear Strength/N/m	247	258	253	221

As can be seen from tables 1 and 2, the polyether polyol prepared by the invention has good openness when used as main polyether under different formula systems and different foam densities, the openness of the foam is 75.6% at most, the tensile strength and the tearing strength are obviously improved, the low-temperature sensitivity coefficient is tested, the comparative proportion is obviously reduced, and the foam is soft, comfortable and not hard under the low-temperature condition.

Claims

1. The polyether polyol for the self-opening low-temperature soft slow-rebound mattress foam is characterized in that: is prepared by copolymerizing an initiator A, an initiator B and alkylene oxide under the action of a catalyst, wherein,

the initiator B is one of propylene glycol, glycerol or pentaerythritol;

the alkylene oxide is propylene oxide and ethylene oxide;

2. The polyether polyol for self-opening, low temperature soft slow rebound mattress foam of claim 1 wherein: the catalyst is one of a phosphazene catalyst, a double metal cyanide complex catalyst or KOH.

3. A process for preparing a polyether polyol for self-opening, low temperature, soft, slow rebound mattress foam of claim 1 or 2 wherein: the method comprises the following steps:

4. A slow rebound foam prepared from the polyether polyol for self-opening, low temperature soft slow rebound mattress foam of claim 1 or 2 wherein: consists of A, B components in a certain proportion,

wherein:

polyether polyol 1 is INOVOL F5631;

5. The slow rebound foam of claim 4, wherein: the polymer polyol is POP 2045.

6. The slow rebound foam of claim 4, wherein: the catalyst is a mixture of A33 and T9.

7. The slow rebound foam of claim 4, wherein: the foam stabilizer is an organic silicon foam stabilizer L580.

8. The slow rebound foam of claim 4, wherein: the foaming agent is water.

9. The slow rebound foam of claim 4, wherein: the mass ratio of the T80 to the DG5412 is 7: 3-8: 2.

10. a method of preparing a slow recovery foam as claimed in any one of claims 4 to 9, wherein: the method comprises the following steps: