阅读说明：本技术 一种季戊四醇聚氧乙烯醚硬脂酸酯的合成方法 (Method for synthesizing pentaerythritol polyoxyethylene ether stearate ) 是由 黎明杰 陈伟钧 彭延平 李玉博 于 2020-04-30 设计创作，主要内容包括：本发明公开了一种季戊四醇聚氧乙烯醚硬脂酸酯的合成方法,包括如下步骤：步骤1：加热熔化：将硬脂酸、季戊四醇聚氧乙烯醚和固定超强酸催化剂投入反应釜中进行加热熔化,其中,季戊四醇聚氧乙烯醚的分子量为5000～9000；直至反应釜内物料全部熔化；步骤2：酯化反应：将步骤1中的物料继续在反应釜中进行酯化反应,直至通过取样测试物料酸值≤15mg·KOH/g；步骤3：冷却过滤：将步骤2中的物料取出反应釜,降温冷却后过滤,得到季戊四醇聚氧乙烯醚硬脂酸酯。通过本发明实现有效提高季戊四醇聚氧乙烯醚硬脂酸酯的合成转化率,满足企业的生产需求。(The invention discloses a method for synthesizing pentaerythritol polyoxyethylene ether stearate, which comprises the following steps: step 1: heating and melting: putting stearic acid, pentaerythritol polyoxyethylene ether and a fixed super acid catalyst into a reaction kettle for heating and melting, wherein the molecular weight of the pentaerythritol polyoxyethylene ether is 5000-9000; until the materials in the reaction kettle are completely melted; step 2: esterification reaction: continuing carrying out esterification reaction on the material in the step 1 in a reaction kettle until the acid value of the material is less than or equal to 15mg KOH/g through sampling test; and step 3: cooling and filtering: and (3) taking the materials in the step (2) out of the reaction kettle, cooling, and filtering to obtain the pentaerythritol polyoxyethylene ether stearate. The invention effectively improves the synthesis conversion rate of the pentaerythritol polyoxyethylene ether stearate and meets the production requirements of enterprises.)

1. A method for synthesizing pentaerythritol polyoxyethylene ether stearate is characterized by comprising the following steps: the method comprises the following steps:

step 1: heating and melting: putting stearic acid, pentaerythritol polyoxyethylene ether and a fixed super acid catalyst into a reaction kettle for heating and melting, wherein the molecular weight of the pentaerythritol polyoxyethylene ether is 5000-9000; until the materials in the reaction kettle are completely melted;

step 2: esterification reaction: continuing carrying out esterification reaction on the material in the step 1 in a reaction kettle until the acid value of the material is less than or equal to 15mg KOH/g through sampling test;

and step 3: cooling and filtering: and (3) taking the materials in the step (2) out of the reaction kettle, cooling, and filtering to obtain the pentaerythritol polyoxyethylene ether stearate.

2. The method for synthesizing pentaerythritol polyoxyethylene ether stearate according to claim 1, wherein the method comprises the following steps: in step 1, the amount of pentaerythritol polyoxyethylene ether added is (amount of stearic acid added × molecular weight of pentaerythritol polyoxyethylene ether)/(284 × 4).

3. The method for synthesizing pentaerythritol polyoxyethylene ether stearate according to claim 1, wherein the method comprises the following steps: in the step 1, the addition amount of the solid super acidic catalyst is (the addition amount of stearic acid + the addition amount of pentaerythritol polyoxyethylene ether) × (1-2%).

4. The method for synthesizing pentaerythritol polyoxyethylene ether stearate according to claim 1, wherein the method comprises the following steps: in the step 1, the heating temperature of the reaction kettle is 100-120 ℃, the stirring speed of the reaction kettle is 80-200 r/min, and the reaction kettle is vacuumized to a negative pressure of more than-0.95 MPa.

5. The method for synthesizing pentaerythritol polyoxyethylene ether stearate according to claim 1, wherein the method comprises the following steps: in the step 2, the heating temperature of the reaction kettle is 180-250 ℃, and nitrogen is slightly introduced into the kettle bottom to maintain the negative pressure above-0.95 MPa.

6. The method for synthesizing pentaerythritol polyoxyethylene ether stearate according to claim 1, wherein the method comprises the following steps: and cooling to 100-120 ℃ in the step 3.

7. The method for synthesizing pentaerythritol polyoxyethylene ether stearate according to claim 1, wherein the method comprises the following steps: the preparation method of the pentaerythritol polyoxyethylene ether in the step 1 comprises the following steps: the pentaerythritol polyoxyethylene ether is prepared by taking commercially available pentaerythritol as a raw material, adding one or more of an epoxy basic catalyst and an acid catalyst, and taking ethylene oxide as a chain extender.

8. The method for synthesizing pentaerythritol polyoxyethylene ether stearate according to any one of claims 1 to 3, wherein: the solid super acid catalyst in the step 1 is one or more of SO42-/Fe2O3, SO42-/ZrO2, SO42-/TiO2, SO42-/TiO2-ZrO2, SO42-/TiO2-SnO2, SO42-/TiO2-La2O3 and MoO3/TiO 2.

Technical Field

The invention relates to the field of preparation of high molecular compounds, and in particular relates to a synthesis method of pentaerythritol polyoxyethylene ether stearate.

Background

The thickening agent is a novel functional polymer material which is rapidly developed in recent years, and is mainly used for improving the viscosity or consistency of products. Has the characteristics of small dosage, obvious thickening, convenient use and the like, and is widely applied to industries of cosmetics, food additives, pharmacy, oil extraction, paper making, printing and dyeing, leather processing and the like.

At present, more than 200 thickening agents are used in the daily chemical industry, mainly comprise inorganic salts, surfactants, water-soluble polymers, fatty alcohol fatty acids and the like, can be used for a detergent in the aspect of daily products, enables the product to be transparent, stable, rich in foam, fine and smooth in hand feeling and easy to rinse, and is also frequently applied to cosmetics, toothpaste and the like. The thickener is a skeleton structure and a core foundation of a product formula in the daily chemical industry, and is important for appearance, rheological property, stability, skin feel and the like of the product. In addition, the water-soluble high molecular weight compound is used as a thickening agent, a suspending agent, a dispersing agent, a shaping agent and the like in the daily chemical industry, is a substance which can improve the viscosity of a product, the stability of the product and the rheological form of the product, and plays important roles in thickening, stabilizing, emulsifying, suspending, retaining water and the like.

The pentaerythritol polyoxyethylene ether stearate is one of thickening agents, and in the field of cosmetics, the pentaerythritol polyoxyethylene ether stearate is a high-molecular-weight composite vegetable oil, is a novel nonionic liquid emulsifier which is suitable for an aqueous cleaning system and has excellent performance, has a thickening effect, has shear rheology, and does not affect foams and skin feel after use.

At present, the synthesis conversion rate of pentaerythritol polyoxyethylene ether stearate is not high, and the production requirements of enterprises are difficult to meet.

Disclosure of Invention

The invention aims to design a synthesis method of pentaerythritol polyoxyethylene ether stearate, which effectively improves the synthesis conversion rate of the pentaerythritol polyoxyethylene ether stearate and meets the production requirements of enterprises.

In order to achieve the purpose, the invention provides the following technical scheme:

a method for synthesizing pentaerythritol polyoxyethylene ether stearate comprises the following steps:

step 1: heating and melting: putting stearic acid, pentaerythritol polyoxyethylene ether and a fixed super acid catalyst into a reaction kettle for heating and melting, wherein the molecular weight of the pentaerythritol polyoxyethylene ether is 5000-9000; until the materials in the reaction kettle are completely melted;

step 2: esterification reaction: continuing carrying out esterification reaction on the material in the step 1 in a reaction kettle until the acid value of the material is less than or equal to 15mg KOH/g through sampling test;

and step 3: cooling and filtering: and (3) taking the materials in the step (2) out of the reaction kettle, cooling, and filtering to obtain the pentaerythritol polyoxyethylene ether stearate.

Preferably, the amount of addition of pentaerythritol polyoxyethylene ether in step 1 ═ (amount of addition of stearic acid × molecular weight of pentaerythritol polyoxyethylene ether)/(284 × 4), with the result that rounding remains to an integer.

Preferably, the solid super acid catalyst is added in step 1 in an amount of × (1-2%) with stearic acid added and pentaerythritol polyoxyethylene ether added, and the result is rounded off and retained as an integer.

Preferably, the heating temperature of the reaction kettle in the step 1 is 100-120 ℃, the stirring speed of the reaction kettle is 80-200 r/min, and the reaction kettle is vacuumized to a negative pressure of more than-0.95 MPa.

Preferably, the heating temperature of the reaction kettle in the step 2 is 180-250 ℃, and nitrogen is slightly introduced into the kettle bottom to maintain the negative pressure above-0.95 MPa.

Preferably, the temperature in the step 3 is reduced to 100-120 ℃.

Preferably, the preparation method of pentaerythritol polyoxyethylene ether in step 1 comprises the following steps: the pentaerythritol polyoxyethylene ether is prepared by taking commercially available pentaerythritol as a raw material, adding one or more of an epoxy basic catalyst and an acid catalyst, and taking ethylene oxide as a chain extender.

Preferably, the solid super acid catalyst in the step 1 is one or more of SO42-/Fe2O3, SO42-/ZrO2, SO42-/TiO2, SO42-/TiO2-ZrO2, SO42-/TiO2-SnO2, SO42-/TiO2-La2O3 and MoO3/TiO 2.

Compared with the prior art, the invention has the beneficial effects that:

the invention effectively improves the synthesis conversion rate of the pentaerythritol polyoxyethylene ether stearate, and the synthesis conversion rate of the pentaerythritol polyoxyethylene ether stearate reaches more than 90 percent. Meanwhile, the solid super acidic catalyst has better catalytic activity, selectivity and reusability for a plurality of chemical reactions, so that the solid super acidic catalyst can be reused for 5-8 times in the synthesis of pentaerythritol polyoxyethylene ether stearate, and is beneficial to environmental protection.

Detailed Description