Preparation method of sucrose polyether with high degree of functionality

Abstract

The invention relates to a preparation method of sucrose polyether with high degree of functionality, and belongs to the technical field of preparation of polyether polyol. The preparation method of the sucrose polyether with high degree of functionality comprises the following steps of using a mixture of sucrose and polyol as an initiating agent, and performing loop-opening reaction with propylene epoxide under the condition of an alkaline catalyst, so as to obtain the sucrose polyether with high degree of functionality. The preparation method has the advantages that the preparation method isscientific and reasonable, the operation is simple, the implementing is easy, the degree of functionality of the polyether is effectively increased, the cost of the raw material is reduced at the same time, and the sucrose polyether can be widely applied to hard foam combining materials; the sucrose polyether can be continuously produced, the demolding time is short, the strength is high, and thesize stability is good.

Description

technical field

[0001] The invention relates to a preparation method of high-functionality sucrose polyether, which belongs to the technical field of preparation of polyether polyols. Background technique

[0002] With the development of the market, the field of polyurethane rigid foam has higher requirements for the functionality of the basic polyether in the composite material. Because in general, the higher the functionality of the base polyether, the better the low temperature dimensional stability of the resulting foam. In fields such as the production of refrigerators that require high foam bulk density, the physical properties of the foam are also required to have high strength and good dimensional stability, and to have sufficient strength under low density conditions.

[0003] When preparing high-functionality polyether polyols in the prior art, the residue of sucrose monomers in the polyether is the biggest difficulty, that is, the conversion rate of sucrose. Co...

Examples

Embodiment 1

[0024] Put 1102g of sucrose (solid), 342g of diethylene glycol, and 6g of sodium hydroxide into a 5L 1# reactor, replace with nitrogen 10 times, and stir when the temperature rises to 80°C to fully fuse the initiator for 1.5h. Vacuum at -0.09MPa, when the temperature is gradually raised to 90°C, 50g of propylene oxide is used for pre-dropping, and when the temperature is continued to rise to 110°C, 2506g of propylene oxide is used for reaction, the reaction pressure is 0.25MPa, and the reaction time is 7h. After the reaction, mature for 3 hours, turn on vacuum and open bubbling to remove the monomer for 2 hours to obtain a reaction solution.

[0025] Most of this reaction solution is discharged into the 2# kettle for aftertreatment, and 500g of the reaction solution remains in the 1# kettle as one of the initiators of the second batch of reactions.

[0026] The 2# kettle was neutralized with phosphoric acid to make the pH = 5.2, 1.0g of magnesium silicate was added, the temper...

Embodiment 2

[0030] Put 954g of sucrose (solid), 327g of glycerin, and 6g of potassium hydroxide into a 5L 1# reactor, replace with nitrogen 10 times, and stir when the temperature rises to 90°C to fully fuse the initiator for 1.5h. Vacuum at -0.09MPa, when the temperature is gradually raised to 95°C, 50g of propylene oxide is used for pre-dropping, and when the temperature is continued to rise to 120°C, 2670g of propylene oxide is used for reaction, the reaction pressure is 0.3MPa, and the reaction time is 6h. After the reaction, mature for 3 hours, turn on vacuum and open bubbling to remove the monomer for 2 hours to obtain a reaction solution.

[0031] Most of this reaction solution is discharged into the 2# kettle for aftertreatment, and 500g of the reaction solution remains in the 1# kettle as one of the initiators of the second batch of reactions.

[0032] The 2# tank was neutralized with phosphoric acid to make the pH = 5.0, 1.2g of magnesium silicate was added, the temperature was ...

Embodiment 3

[0036] Put 1127g of sucrose (solid) and 234g of propylene glycol into a 5L 1# reactor, replace with nitrogen 10 times, suck in 32g of dimethylamine under negative pressure, and stir when the temperature rises to 80°C to fully fuse the initiator for 1 hour. When the temperature is gradually raised to 80°C, 50g of propylene oxide is used for pre-dropping. When the temperature continues to rise to 95°C, 1290g of propylene oxide is used for the reaction. The reaction pressure is 0.3MPa. , Reaction pressure 0.3MPa, reaction time 9h. After the reaction, mature for 3 hours, turn on vacuum and open bubbling to remove the monomer for 2 hours to obtain a reaction solution.

[0037] Most of this reaction solution is discharged into the 2# kettle for aftertreatment, and 500g of the reaction solution remains in the 1# kettle as one of the initiators of the second batch of reactions.

[0038] The 2# tank was neutralized with oxalic acid to make the pH=5.4, 1.1g of magnesium silicate was ad...

technical field

[0001] The invention relates to a preparation method of high-functionality sucrose polyether, which belongs to the technical field of preparation of polyether polyols. Background technique

[0002] With the development of the market, the field of polyurethane rigid foam has higher requirements for the functionality of the basic polyether in the composite material. Because in general, the higher the functionality of the base polyether, the better the low temperature dimensional stability of the resulting foam. In fields such as the production of refrigerators that require high foam bulk density, the physical properties of the foam are also required to have high strength and good dimensional stability, and to have sufficient strength under low density conditions.

[0003] When preparing high-functionality polyether polyols in the prior art, the residue of sucrose monomers in the polyether is the biggest difficulty, that is, the conversion rate of sucrose. Co...

Examples

Embodiment 1

[0024] Put 1102g of sucrose (solid), 342g of diethylene glycol, and 6g of sodium hydroxide into a 5L 1# reactor, replace with nitrogen 10 times, and stir when the temperature rises to 80°C to fully fuse the initiator for 1.5h. Vacuum at -0.09MPa, when the temperature is gradually raised to 90°C, 50g of propylene oxide is used for pre-dropping, and when the temperature is continued to rise to 110°C, 2506g of propylene oxide is used for reaction, the reaction pressure is 0.25MPa, and the reaction time is 7h. After the reaction, mature for 3 hours, turn on vacuum and open bubbling to remove the monomer for 2 hours to obtain a reaction solution.

[0025] Most of this reaction solution is discharged into the 2# kettle for aftertreatment, and 500g of the reaction solution remains in the 1# kettle as one of the initiators of the second batch of reactions.

[0026] The 2# kettle was neutralized with phosphoric acid to make the pH = 5.2, 1.0g of magnesium silicate was added, the temper...

Embodiment 2

[0030] Put 954g of sucrose (solid), 327g of glycerin, and 6g of potassium hydroxide into a 5L 1# reactor, replace with nitrogen 10 times, and stir when the temperature rises to 90°C to fully fuse the initiator for 1.5h. Vacuum at -0.09MPa, when the temperature is gradually raised to 95°C, 50g of propylene oxide is used for pre-dropping, and when the temperature is continued to rise to 120°C, 2670g of propylene oxide is used for reaction, the reaction pressure is 0.3MPa, and the reaction time is 6h. After the reaction, mature for 3 hours, turn on vacuum and open bubbling to remove the monomer for 2 hours to obtain a reaction solution.

[0031] Most of this reaction solution is discharged into the 2# kettle for aftertreatment, and 500g of the reaction solution remains in the 1# kettle as one of the initiators of the second batch of reactions.

[0032] The 2# tank was neutralized with phosphoric acid to make the pH = 5.0, 1.2g of magnesium silicate was added, the temperature was ...

Embodiment 3

[0036] Put 1127g of sucrose (solid) and 234g of propylene glycol into a 5L 1# reactor, replace with nitrogen 10 times, suck in 32g of dimethylamine under negative pressure, and stir when the temperature rises to 80°C to fully fuse the initiator for 1 hour. When the temperature is gradually raised to 80°C, 50g of propylene oxide is used for pre-dropping. When the temperature continues to rise to 95°C, 1290g of propylene oxide is used for the reaction. The reaction pressure is 0.3MPa. , Reaction pressure 0.3MPa, reaction time 9h. After the reaction, mature for 3 hours, turn on vacuum and open bubbling to remove the monomer for 2 hours to obtain a reaction solution.

[0037] Most of this reaction solution is discharged into the 2# kettle for aftertreatment, and 500g of the reaction solution remains in the 1# kettle as one of the initiators of the second batch of reactions.

[0038] The 2# tank was neutralized with oxalic acid to make the pH=5.4, 1.1g of magnesium silicate was ad...