阅读说明：本技术 一种鞋材专用分散剂的制备方法 (Preparation method of special dispersing agent for shoe materials ) 是由 连江斌 连嘉杰 陈惠香 于 2019-09-19 设计创作，主要内容包括：本发明公开了一种鞋材专用分散剂的制备方法,分散剂采用高活性原材料以及多官能度基础聚醚,具体包括脱水、酯化反应、测氧含量、催化剂加入、测氧含量以及封端反应等步骤研制出鞋材专用分散剂,不但可以提高产品反应活性、分散性及硬度,满足不断提高的下游客户要求,适合用于整个聚氨酯鞋材行业。(The invention discloses a preparation method of a special dispersing agent for shoe materials, wherein the dispersing agent adopts high-activity raw materials and multifunctional basic polyether, and specifically comprises the steps of dehydration, esterification reaction, oxygen content measurement, catalyst addition, oxygen content measurement, end capping reaction and the like, so that the special dispersing agent for shoe materials is developed, the reaction activity, the dispersibility and the hardness of products can be improved, the continuously improved downstream customer requirements can be met, and the special dispersing agent is suitable for the whole polyurethane shoe material industry.)

1. A preparation method of a special dispersing agent for shoe materials is characterized in that the dispersing agent adopts high-activity raw materials and multifunctional basic polyether, and specifically comprises the following steps:

Step one, dehydration: and (3) putting 88-95 parts by weight of high-activity polyether into an intermittent kettle, heating for dehydration at the temperature of 100 ℃ and 120 ℃, under the pressure of less than or equal to-0.093 MPa, and testing the moisture once every 2 hours, wherein the moisture content is less than or equal to 0.05 percent, and the product is qualified.

Step two, esterification reaction: cooling the material to 40-60 ℃, adding 0.5-5 parts by weight of maleic anhydride, bubbling nitrogen for half an hour at the pressure of 0.02-0.2MPa and at the temperature of 40-60 ℃.

Step three, measuring the oxygen content: less than or equal to 100 PPm.

Step four, adding a catalyst: the temperature is controlled at 125-135 ℃, the pressure is released at the beginning of timing, the pressure release time is 2 hours, the pressure is released to the normal pressure, and 0.01 to 0.05 weight part of catalyst is poured into the reactor through a feeding opening.

Step five, measuring the oxygen content: less than or equal to 100 PPm.

Step six, end-capping reaction: firstly, pressure is relieved to 0.02-0.04 Mpa; then adding 3-9 parts by weight of ethylene oxide, wherein the pressure is less than or equal to 0.4Mpa, and the temperature is as follows: 120 ℃ and 135 ℃; internal pressure 10 hours, temperature: at the temperature of 120 ℃ and 135 ℃, the pressure is less than or equal to 0.43 MPa; the prepared product is light yellow-amber, and the acid value and the viscosity of the finished product are measured.

2. The preparation method of the special dispersing agent for shoe materials according to claim 1, characterized by comprising the following steps: the high-activity polyether in the step one has a functionality of 4-8.

3. The preparation method of the special dispersing agent for shoe materials according to claim 1, characterized by comprising the following steps: and the catalyst in the fourth step is one of divalent metal oxide, divalent metal naphthenate and quaternary ammonia base.

Technical Field

The invention relates to a preparation method of a dispersing agent, in particular to a special dispersing agent for shoe materials.

Background

The shoe industry in China is different from military projects, the shoe industry presents a strong development situation in more than ten years of shortness, China is the largest shoe manufacturing production area in the world, and a very complete industrial chain and industrial development platform are provided at present. The shoe industry in China already shows an industry cluster type development state.

Therefore, the special dispersing agent for shoe materials has very considerable market prospect, and accounts for about 5 percent of the total amount of polyether. In recent years, the market of polyurethane stock solution in China is influenced by the price of raw materials, the growth speed is slowed down, and the proportion of the existing polyurethane shoe materials is less than 6 percent, so the market space of the existing polyurethane shoe materials is still large. In addition, because the industrial entry threshold of polyether is low, the production capacity of polyether is rapidly expanded, and therefore, the polyether market has a serious problem of over-supply.

At present, the technology of the special dispersing agent for shoe materials in the market is not mature enough, equipment is old, the device is backward, products are frequently switched, and the product quality is unstable. Starting from the raw materials, the quality of the product is improved, and the product is more competitive in the market.

Disclosure of Invention

The invention aims to overcome the defects in the prior art and provides a preparation method of a special dispersing agent for shoe materials.

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

A preparation method of a special dispersing agent for shoe materials, wherein the dispersing agent adopts high-activity raw materials and multifunctional basic polyether, and specifically comprises the following steps:

Step one, dehydration: and (3) putting 88-95 parts by weight of high-activity polyether into an intermittent kettle, heating for dehydration at the temperature of 100 ℃ and 120 ℃, under the pressure of less than or equal to-0.093 MPa, and testing the moisture once every 2 hours, wherein the moisture content is less than or equal to 0.05 percent, and the product is qualified.

Step two, esterification reaction: cooling the material to 40-60 ℃, adding 0.5-5 parts by weight of maleic anhydride, bubbling nitrogen for half an hour at the pressure of 0.02-0.2MPa and at the temperature of 40-60 ℃.

Step three, measuring the oxygen content: less than or equal to 100 PPm.

Step four, adding a catalyst: the temperature is controlled at 125-135 ℃, the pressure is released at the beginning of timing, the pressure release time is 2 hours, the pressure is released to the normal pressure, and 0.01 to 0.05 weight part of catalyst is poured into the reactor through a feeding opening.

Step five, measuring the oxygen content: less than or equal to 100 PPm.

Step six, end-capping reaction: firstly, pressure is relieved to 0.02-0.04 Mpa; then adding 3-9 parts by weight of ethylene oxide, wherein the pressure is less than or equal to 0.4Mpa, and the temperature is as follows: 120 ℃ and 135 ℃; internal pressure 10 hours, temperature: at the temperature of 120 ℃ and 135 ℃, the pressure is less than or equal to 0.43 MPa; the prepared product is light yellow-amber, and the acid value and the viscosity of the finished product are measured.

preferably, the high activity polyether of step one is selected from those having a functionality of 4 to 8.

Preferably, the catalyst in the fourth step is one of a divalent metal oxide, a divalent metal naphthenate and a quaternary ammonia base.

As can be seen from the above description, the present invention has advantages compared with the prior art:

1. The high-activity multifunctional polyether is selected, the hardness of the product is effectively improved, the basic polyether reacts with ethylene oxide, and the prepared dispersing agent containing the induced unsaturated double bond can improve the performance of the dispersing agent, reduce the viscosity of the product and reduce the cost of customers;

2. the polyether and the ethylene oxide with high activity can effectively improve the reaction activity of the product, improve the conversion rate of the product, have low residual monomer and reduce the pressure of environmental protection.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The special dispersing agent for the shoe material comprises the following raw material components in parts by weight:

high-activity polyether: 88-95 parts, maleic anhydride: 0.5-5 parts of catalyst: 0.01-0.05 part, ethylene oxide: 3-9 parts.

The high-activity polyether in the step one has a functionality of 4-8.

And the catalyst in the fourth step is one of divalent metal oxide, divalent metal naphthenate and quaternary ammonia base.