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Preparation method of controllable-composition polyoxyethylene sorbitol (sorbitan) fatty acid ester
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A technology of sorbitan and polyoxyethylene, which is applied in the field of preparation of polyoxyethylene sorbitan fatty acid esters, can solve problems such as incomplete preparation, and achieve stable quality and high product purity
Inactive Publication Date: 2015-02-25
NANJING WELL CHEM
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These four patents are limited to the preparation of polysorbate 80 by the method of the present invention or similar to the present invention, and cannot fully solve the problem of preparation of polyoxyethylene (anhydrous) sorbitan fatty acid ester products with controllable structure and composition
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Embodiment 1～4
[0055] [embodiment 1~4] the preparation of polyoxyethylene sorbitol ether
[0056] In the 3L stainless steel autoclave, add the sorbitol (purity ≥ 99%) of the amount shown in Table 1, catalyst, after replacing with nitrogen, be warming up to 90 ℃, then slowly pressurize the oxirane of the amount shown in Table 1 with nitrogen Put it into an autoclave for addition polymerization reaction, control the addition rate of ethylene oxide, maintain the temperature of the kettle at 140°C to 150°C, and the pressure at 0.4MPa. After adding the ethylene oxide, aging for 2h, the pressure in the kettle is reduced to normal pressure, and the temperature is lowered. to 70-80°C, treated with synthetic magnesium silicate with 1% mass of reactant for 1 h, filtered to obtain polyoxyethylene sorbitol ether, measured and measured for hydroxyl value, the results are listed in Table 1.
[0057] The preparation result of table 1 polyoxyethylene sorbitol ether
[0058]
[0059] *The catalyst is sod...
Embodiment 5～8
[0060] [Examples 5-8] Preparation of Polyoxyethylene-Sorbitan Ether
[0061] It is basically the same as Example 1, but the sorbitol is changed into 1,4-sorbitol (purity ≥ 99%), and the feeding amount of it and ethylene oxide and the yield and hydroxyl value of the product are shown in Table 2.
[0062] The preparation result of table 2 polyoxyethylene-sorbitan ether
[0063]
[0064] *The catalyst is sodium hydroxide.
Embodiment 9～12
[0065] [Examples 9-12] Preparation of Polyoxyethylene Isosorbide
[0066] Substantially the same as Example 1, but changing sorbitol into isosorbide (purity ≥ 99%), its charging amount and product yield and hydroxyl value of ethylene oxide are shown in Table 3.
[0067] The preparation result of table 3 polyoxyethylene isosorbide
[0068]
[0069]
[0070] *The catalyst is potassium hydroxide.
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Abstract
The invention discloses a preparation method of controllable-composition polyoxyethylene sorbitol (sorbitan) fatty acid ester, which comprises the following steps: proportionally mixing one or at least two or three of high-purity sorbitol (II), high-purity 1,4-sorbitan (III) and high-purity 1,4,3,6-sorbitan (IV, isosorbitol) to obtain a mixture (V), polymerizing with epoxyethane under the action of an alkaline catalyst, and refining by using a refining agent at a certain refinement temperature to obtain high-purity polyoxyethylene sorbitol (sorbitan) ether (VI); and esterifying with fatty acid under the action of a high-efficiency composite esterification catalyst, and adsorbing by an adsorbent to obtain the high-purity polyoxyethylene sorbitol (sorbitan) fatty acid ester (I). The method solves the problem of generality in the preparation of the polyoxyethylene sorbitol (sorbitan) fatty acid ester, and ensures the controllability on composition and quality of the product, thereby greatly enhancing the use safety.
Description
technical field [0001] The invention relates to a preparation method of polyoxyethylene (anhydrous) sorbitan fatty acid ester with controllable composition, belonging to the field of chemical synthesis. technical background [0002] Polyoxyethylene (anhydrous) sorbitan fatty acid ester contains hydrophilic group polyoxyethylene chain and lipophilic group ester group, has good emulsifying and solubilizing ability, and has been widely used in textile, food and other industries. In the field of medicine, such compounds, such as polysorbate 20, polysorbate 40, polysorbate 60, and polysorbate 80, can be used as emulsifiers and solubilizers for insoluble drugs. High-purity polysorbate can be used as a solubilizer for injection preparations and is an important pharmaceutical excipient. [0003] Patent CN102585198A discloses a preparation method of polysorbate not containing polyoxyethylene fatty acid ester of isosorbide. The method uses sorbitol as raw material, and directly este...
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