Preparation method for polyester polyol by grease restructuring

Abstract

The invention discloses a preparation method for polyester polyol by grease restructuring, comprising the following steps: carrying out a basic hydrolysis on grease raw materials to prepare aliphatic acid and glycerin; weighing to take certain mass proportion of aliphatic acid, acetate, hydrogen peroxide (30%) and a catalyst, wherein m aliphatic acid: m acetate : m hydrogen peroxide : m sulfuric acid = 100:0-50:40-150:1-5, and adding the aliphatic acid, acetate and the catalyst into a reactor simultaneously; adding the hydrogen peroxide dropwisely for 1 hour to 2 hours at a temperature of 40 DEG C, standing the mixture for reaction for 2 to 4 hours at a temperature of 60 DEG C, and carrying our a ring opening hydrolysis for 1 hour to 2 hours in backflow state; carrying out phase splittingon the oxidized product, adding glycerin and an esterification catalyst into the organic phase, and carrying out esterification for 1 hour to 2 hours at a temperature of 180 DEG C under the conditionof reduced pressure (5-10 Kpa). Therefore, aliphatic acid polyester polyol with an acid value of 1 to 10 mg KOH / g and a hydroxyl value of 280 to 410 mg KOH / g is obtained.

Description

technical field

[0001] The invention belongs to the field of biomass material preparation, and mainly relates to the preparation of environmentally friendly polyester polyol for foaming. Background technique

[0002] The preparation of grease-based polyols in current patents is mainly the direct transesterification method, such as (CN101747497A, CN101602665,) and the like. These methods only rely on polyols to introduce hydroxyl groups, the hydroxyl value is low, and the controllable range is small. From a structural point of view, transesterification can only connect hydroxyl groups to one side of the fatty acid. Such polyols have certain defects in foaming performance, and it is difficult to form a three-dimensional structure. Therefore, they must be used in conjunction with other polyols. Contents of the invention

[0003] In order to solve the defect that the oil-based polyols in the prior art are difficult to form a three-dimensional structure when foaming, the p...

Examples

Embodiment 1

[0026] In the first step, put soybean oil and NaOH into a three-necked flask together with 25ml of distilled water according to the ratio of n (fat): n (NaOH) = 1:1.1, mechanically stir evenly, react at 70°C for 1.5h, keep warm for 2h, and cool After reaching room temperature, add hydrochloric acid dropwise to a pH value of 3-4, continue to keep warm at room temperature for 1 hour, let stand to separate layers, the upper oil phase is rotary evaporated to obtain fatty acid, the lower layer water phase is rotary evaporated to remove water, and then collected under reduced pressure of 0.095MPa The product at 180-200°C is glycerin.

[0027] The second step, according to the mass ratio m 脂肪酸 : m 乙酸 :m 双氧水 :m 环氧化催化剂 =100:10:60:2 ratio, weigh fatty acid, acetic acid, hydrogen peroxide (30%) and concentrated sulfuric acid, and add fatty acid, acetic acid and catalyst into the reactor at the same time. Add hydrogen peroxide dropwise at 40°C for 1.5h, then react at 60°C for 3h, and ...

Embodiment 2-5

[0030] Except the following differences, others are the same as Example 1

[0031] Example

Embodiment 6-7

[0033] Except the following differences, others are the same as Example 1

[0034] Example

technical field

[0001] The invention belongs to the field of biomass material preparation, and mainly relates to the preparation of environmentally friendly polyester polyol for foaming. Background technique

[0002] The preparation of grease-based polyols in current patents is mainly the direct transesterification method, such as (CN101747497A, CN101602665,) and the like. These methods only rely on polyols to introduce hydroxyl groups, the hydroxyl value is low, and the controllable range is small. From a structural point of view, transesterification can only connect hydroxyl groups to one side of the fatty acid. Such polyols have certain defects in foaming performance, and it is difficult to form a three-dimensional structure. Therefore, they must be used in conjunction with other polyols. Contents of the invention

[0003] In order to solve the defect that the oil-based polyols in the prior art are difficult to form a three-dimensional structure when foaming, the p...

Examples

Embodiment 1

[0026] In the first step, put soybean oil and NaOH into a three-necked flask together with 25ml of distilled water according to the ratio of n (fat): n (NaOH) = 1:1.1, mechanically stir evenly, react at 70°C for 1.5h, keep warm for 2h, and cool After reaching room temperature, add hydrochloric acid dropwise to a pH value of 3-4, continue to keep warm at room temperature for 1 hour, let stand to separate layers, the upper oil phase is rotary evaporated to obtain fatty acid, the lower layer water phase is rotary evaporated to remove water, and then collected under reduced pressure of 0.095MPa The product at 180-200°C is glycerin.

[0027] The second step, according to the mass ratio m 脂肪酸 : m 乙酸 :m 双氧水 :m 环氧化催化剂 =100:10:60:2 ratio, weigh fatty acid, acetic acid, hydrogen peroxide (30%) and concentrated sulfuric acid, and add fatty acid, acetic acid and catalyst into the reactor at the same time. Add hydrogen peroxide dropwise at 40°C for 1.5h, then react at 60°C for 3h, and ...

Embodiment 2-5

[0030] Except the following differences, others are the same as Example 1

[0031] Example

Embodiment 6-7

[0033] Except the following differences, others are the same as Example 1

[0034] Example

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