阅读说明：本技术 一种十八脂肪胺聚氧乙烯醚的制备方法 (Preparation method of octadecyl amine polyoxyethylene ether ) 是由 韩军 潘永清 于 2020-05-22 设计创作，主要内容包括：一种十八脂肪胺聚氧乙烯醚的制备方法,包括以下步骤：向反应釜内通入氮气；将部分十八脂肪胺加入反应釜内；打开化工泵；向反应釜内加入部分雾化状态的环氧乙烷；开启搅拌装置；调整化工泵的物料流速；向反应釜内部加入氢氧化钾以及其余全部量的十八脂肪胺；向反应釜内加入部分雾化状态的环氧乙烷；反应釜保温30分钟后,冷却出料。本发明中,实现物料在反应釜内部的循环流动,提高物料之间的混合均匀程度,保证物料之间的充分混合,提高产品质量。(A preparation method of octadecyl amine polyoxyethylene ether comprises the following steps: introducing nitrogen into the reaction kettle; adding part of the octadecylamine into a reaction kettle; opening a chemical pump; adding part of atomized ethylene oxide into the reaction kettle; starting the stirring device; adjusting the material flow rate of the chemical pump; adding potassium hydroxide and the rest of the total amount of the octadecylamine into the reaction kettle; adding part of atomized ethylene oxide into the reaction kettle; and (5) keeping the temperature of the reaction kettle for 30 minutes, cooling and discharging. According to the invention, the materials can circularly flow in the reaction kettle, the uniform mixing degree of the materials is improved, the materials are fully mixed, and the product quality is improved.)

1. A preparation method of octadecyl amine polyoxyethylene ether is characterized by comprising the following steps:

s1: introducing nitrogen into the reaction kettle to discharge air in the reaction kettle;

s2: adding part of octadecylamine into a reaction kettle, and heating to 170-180 ℃; the part of the octadecyl amine accounts for 40 percent of the total mass of the octadecyl amine;

s3: opening a chemical pump, pumping out the material at the bottom of the reaction kettle, and inputting the material into the reaction kettle from a discharge pipe at the top of the reaction kettle; lasting for five minutes to ensure that the internal temperature of the reaction kettle is constant;

s4: adding part of atomized ethylene oxide into the reaction kettle, wherein the atomized ethylene oxide enters the reaction kettle from an air inlet pipe at the bottom of the reaction kettle; the part of ethylene oxide accounts for 30% of the total mass of the ethylene oxide;

s5: starting a stirring device to stir the materials in the reaction kettle;

s6: adjusting the material flow rate of the chemical pump, wherein the material flow rate is 200-;

s7: reacting the materials in the reaction kettle for 1-2 hours, closing the chemical pump after the reaction is finished, and continuously stirring by the stirring device until the temperature of the materials is cooled to 75-85 ℃;

s8: adding potassium hydroxide and the rest of the total amount of octadecylamine into the reaction kettle, heating to 110-;

s9: adding part of atomized ethylene oxide into the reaction kettle, wherein the atomized ethylene oxide enters the reaction kettle from an air inlet pipe at the bottom of the reaction kettle; the part of ethylene oxide accounts for 30% of the total mass of the ethylene oxide; (ii) a

S10: adding part of atomized ethylene oxide into the reaction kettle again; the part of ethylene oxide accounts for 50 percent of the total mass of the ethylene oxide, and the addition of the ethylene oxide is completed within 0.5 to 1 hour;

s11: after each part of materials in the reaction kettle react for 1-1.5 hours, adding the rest of the ethylene oxide in the atomized state into the reaction kettle again, and finishing the addition of the ethylene oxide within 0.3-0.5 hour;

s12: the reaction of the materials in the reaction kettle lasts for 0.5-1 hour, and the chemical pump is closed;

s13: the reaction of the materials in the reaction kettle lasts for 0.5 to 1 hour, and the stirring device is closed;

s14: and (5) keeping the temperature of the reaction kettle for 30 minutes, cooling and discharging.

2. The method for preparing octadecyl amine polyoxyethylene ether according to claim 1, wherein the air inlet pipe is provided with an anti-suck-back U-shaped pipe structure.

3. The method for preparing octadecyl amine polyoxyethylene ether according to claim 1, wherein octadecyl amine accounts for 25-30% of the total mass of the reaction raw materials.

4. The method for preparing octadecyl amine polyoxyethylene ether according to claim 1, wherein the ethylene oxide in atomized state accounts for 65-80% of the total mass of the reaction raw materials.

5. The method for preparing octadecyl amine polyoxyethylene ether according to claim 1, wherein potassium hydroxide accounts for 0.15-0.4% of the total mass of the reaction raw materials.

6. The preparation method of the octadecyl amine polyoxyethylene ether according to claim 1, wherein the stirring device comprises a power device (1), a stirring shaft (2), a spiral pushing piece (3) and a stirring paddle (4);

the stirring shaft (2) is in power connection with the power device, and the stirring shaft (2) is obliquely arranged in the reaction kettle;

the spiral pushing piece (3) is arranged on the periphery of the stirring shaft (2) and is used for transporting materials at the bottom of the reaction kettle to the upper part of the reaction kettle;

the stirring paddle (4) is vertically arranged on the stirring shaft (2) along the direction of the radius of the stirring shaft (2).

Technical Field

The invention relates to the field of chemical product manufacturing, in particular to a preparation method of octadecyl amine polyoxyethylene ether.

Background

At present, the preparation method of the octadecyl amine polyoxyethylene ether adopts a one-step stirring method, wherein the octadecyl amine and ethylene oxide are subjected to polymerization reaction in a stirring reaction kettle, and the catalyst is potassium hydroxide. The polymerization reaction of the octadecylamine and the ethylene oxide is carried out in the material, the polymerization reaction space is small, the material flow in a kettle is poor, the layering phenomenon is serious, the polymerization reaction is greatly influenced by the material, the reaction is incomplete and thorough, and the quality of a finished product is poor.

Disclosure of Invention

Objects of the invention

In order to solve the technical problems in the background art, the invention provides a preparation method of octadecyl amine polyoxyethylene ether, which realizes the circular flow of materials in a reaction kettle, improves the uniform mixing degree of the materials, ensures the sufficient mixing of the materials and improves the product quality.

(II) technical scheme

In order to solve the problems, the invention provides a preparation method of octadecyl amine polyoxyethylene ether, which comprises the following steps:

s1: introducing nitrogen into the reaction kettle to discharge air in the reaction kettle;

s2: adding part of octadecylamine into a reaction kettle, and heating to 170-180 ℃; the part of the octadecyl amine accounts for 40 percent of the total mass of the octadecyl amine;

s3: opening a chemical pump, pumping out the material at the bottom of the reaction kettle, and inputting the material into the reaction kettle from a discharge pipe at the top of the reaction kettle; lasting for five minutes to ensure that the internal temperature of the reaction kettle is constant;

s4: adding part of atomized ethylene oxide into the reaction kettle, wherein the atomized ethylene oxide enters the reaction kettle from an air inlet pipe at the bottom of the reaction kettle; the part of ethylene oxide accounts for 30% of the total mass of the ethylene oxide;

s5: starting a stirring device to stir the materials in the reaction kettle;

s6: adjusting the material flow rate of the chemical pump, wherein the material flow rate is 200-;

s7: reacting the materials in the reaction kettle for 1-2 hours, closing the chemical pump after the reaction is finished, and continuously stirring by the stirring device until the temperature of the materials is cooled to 75-85 ℃;

s8: adding potassium hydroxide and the rest of the total amount of octadecylamine into the reaction kettle, heating to 110-;

s9: adding part of atomized ethylene oxide into the reaction kettle, wherein the atomized ethylene oxide enters the reaction kettle from an air inlet pipe at the bottom of the reaction kettle; the part of ethylene oxide accounts for 30% of the total mass of the ethylene oxide; (ii) a

S10: adding part of atomized ethylene oxide into the reaction kettle again; the part of ethylene oxide accounts for 50 percent of the total mass of the ethylene oxide, and the addition of the ethylene oxide is completed within 0.5 to 1 hour;

s11: after each part of materials in the reaction kettle react for 1-1.5 hours, adding the rest of the ethylene oxide in the atomized state into the reaction kettle again, and finishing the addition of the ethylene oxide within 0.3-0.5 hour;

s12: the reaction of the materials in the reaction kettle lasts for 0.5-1 hour, and the chemical pump is closed;

s13: the reaction of the materials in the reaction kettle lasts for 0.5 to 1 hour, and the stirring device is closed;

s14: and (5) keeping the temperature of the reaction kettle for 30 minutes, cooling and discharging.

Preferably, the air inlet pipe is provided with an anti-suck-back U-shaped pipe structure.

Preferably, the octadecylamine accounts for 25-30% of the total mass of the reaction raw materials.

Preferably, the ethylene oxide in atomized form comprises 65 to 80% by weight of the total mass of the reaction feed.

Preferably, the potassium hydroxide accounts for 0.15-0.4% of the total mass of the reaction raw materials.

Preferably, the stirring device comprises a power device, a stirring shaft, a spiral pushing piece and a stirring paddle; the stirring shaft is in power connection with the power device and is obliquely arranged in the reaction kettle; the spiral pushing piece is arranged on the periphery of the stirring shaft and used for transporting materials at the bottom of the reaction kettle to the upper part of the reaction kettle; the stirring paddle is vertically arranged on the stirring shaft along the direction of the radius of the stirring shaft.

According to the invention, the chemical pump pumps out the material at the bottom of the reaction kettle and inputs the material into the reaction kettle from the discharge pipe at the top of the reaction kettle, so that the material can circularly flow in the reaction kettle, the uniform mixing degree of the materials is improved, and the sufficient mixing of the materials is ensured. And adding part of atomized ethylene oxide into the reaction kettle, wherein the atomized ethylene oxide enters the reaction kettle from an air inlet pipe at the bottom of the reaction kettle, and the ethylene oxide and the octadecylamine are fully contacted and mixed to the maximum extent.

According to the invention, the octadecylamine and the ethylene oxide are gradually added, polymerization is carried out without adding a catalyst, the octadecylamine can be ammoniated better under the conditions of set temperature and pressure, and before polymerization, unsaturated fatty amine is thoroughly opened, so that the reaction is better during polymerization. Then adding catalyst to form liposuction gaps on material molecules, so that the surface area of the liposuction gaps is greatly increased, the surface molecular state is a three-dimensional network structure, and the lipolysis catalyst has excellent thixotropic and dispersing properties, so that the polymerization reaction is more thorough, the chemical stability of the product is good, the product is easy to disperse in water, and the operation is easy, safe and reliable. Meanwhile, materials are added step by step, so that the materials can be fully mixed, and the product quality is improved.

Drawings

FIG. 1 is a schematic structural diagram of a stirring device in the preparation method of octadecyl amine polyoxyethylene ether provided by the invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.

As shown in figure 1, the preparation method of the octadecyl amine polyoxyethylene ether provided by the invention comprises the following steps:

s1: introducing nitrogen into the reaction kettle to discharge air in the reaction kettle;

s2: adding part of octadecylamine into a reaction kettle, and heating to 170-180 ℃; the part of the octadecyl amine accounts for 40 percent of the total mass of the octadecyl amine;

s3: opening a chemical pump, pumping out the material at the bottom of the reaction kettle, and inputting the material into the reaction kettle from a discharge pipe at the top of the reaction kettle; lasting for five minutes to ensure that the internal temperature of the reaction kettle is constant;

s4: adding part of atomized ethylene oxide into the reaction kettle, wherein the atomized ethylene oxide enters the reaction kettle from an air inlet pipe at the bottom of the reaction kettle; the part of ethylene oxide accounts for 30% of the total mass of the ethylene oxide;

s5: starting a stirring device to stir the materials in the reaction kettle;

s6: adjusting the material flow rate of the chemical pump, wherein the material flow rate is 200-;

s7: reacting the materials in the reaction kettle for 1-2 hours, closing the chemical pump after the reaction is finished, and continuously stirring by the stirring device until the temperature of the materials is cooled to 75-85 ℃;

s8: adding potassium hydroxide and the rest of the total amount of octadecylamine into the reaction kettle, heating to 110-;

s9: adding part of atomized ethylene oxide into the reaction kettle, wherein the atomized ethylene oxide enters the reaction kettle from an air inlet pipe at the bottom of the reaction kettle; the part of ethylene oxide accounts for 30% of the total mass of the ethylene oxide; (ii) a

S10: adding part of atomized ethylene oxide into the reaction kettle again; the part of ethylene oxide accounts for 50 percent of the total mass of the ethylene oxide, and the addition of the ethylene oxide is completed within 0.5 to 1 hour;

s11: after each part of materials in the reaction kettle react for 1-1.5 hours, adding the rest of the ethylene oxide in the atomized state into the reaction kettle again, and finishing the addition of the ethylene oxide within 0.3-0.5 hour;

s12: the reaction of the materials in the reaction kettle lasts for 0.5-1 hour, and the chemical pump is closed;

s13: the reaction of the materials in the reaction kettle lasts for 0.5 to 1 hour, and the stirring device is closed;

s14: and (5) keeping the temperature of the reaction kettle for 30 minutes, cooling and discharging.

According to the invention, the chemical pump pumps out the material at the bottom of the reaction kettle and inputs the material into the reaction kettle from the discharge pipe at the top of the reaction kettle, so that the material can circularly flow in the reaction kettle, the uniform mixing degree of the materials is improved, and the sufficient mixing of the materials is ensured. And adding part of atomized ethylene oxide into the reaction kettle, wherein the atomized ethylene oxide enters the reaction kettle from an air inlet pipe at the bottom of the reaction kettle, and the ethylene oxide and the octadecylamine are fully contacted and mixed to the maximum extent.

According to the invention, the octadecylamine and the ethylene oxide are gradually added, polymerization is carried out without adding a catalyst, the octadecylamine can be ammoniated better under the conditions of set temperature and pressure, and before polymerization, unsaturated fatty amine is thoroughly opened, so that the reaction is better during polymerization. Then adding catalyst to form liposuction gaps on material molecules, so that the surface area of the liposuction gaps is greatly increased, the surface molecular state is a three-dimensional network structure, and the lipolysis catalyst has excellent thixotropic and dispersing properties, so that the polymerization reaction is more thorough, the chemical stability of the product is good, the product is easy to disperse in water, and the operation is easy, safe and reliable. Meanwhile, materials are added step by step, so that the materials can be fully mixed, and the product quality is improved.

In an alternative embodiment, the air inlet pipe is provided with an anti-suck-back U-shaped pipe structure, so that materials are prevented from entering the air inlet pipe.

In an alternative embodiment, the octadecylamine comprises 25-30% of the total mass of the reaction feed.

In an alternative embodiment, the ethylene oxide in atomized form comprises 65-80% of the total mass of the reaction feed.

In an alternative embodiment, the potassium hydroxide comprises 0.15-0.4% of the total mass of the reaction feed.

In an alternative embodiment, the stirring device comprises a power device 1, a stirring shaft 2, a spiral pushing piece 3 and a stirring paddle 4; the stirring shaft 2 is in power connection with a power device, and the stirring shaft 2 is obliquely arranged in the reaction kettle; the spiral pushing piece 3 is arranged on the periphery of the stirring shaft 2 and used for transporting materials at the bottom of the reaction kettle to the upper part of the reaction kettle; the stirring paddle 4 is vertically arranged on the stirring shaft 2 along the direction of the radius of the stirring shaft 2.

It should be noted that, agitating unit cooperation chemical industry pump can carry out the mixture and the stirring of dashing the dusk with the inside material of reation kettle to improve the mixture degree of consistency and the mixing efficiency of material, and then improve the quality of product.

It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.