阅读说明：本技术 一种促进剂mbt的提纯工艺 (Purification process of accelerator MBT ) 是由 田少华 张宏亮 魏伟涛 鞠光 王丽敏 于 2019-11-12 设计创作，主要内容包括：本发明涉及促进剂技术领域,具体涉及一种促进剂MBT的提纯工艺,包括以下步骤：步骤一,称取一定量的MBT与氨水,且MBT与氨水的摩尔比为1：3；步骤二,将称取好的MBT和氨水投入反应釜内,按照含固率为20％的加入工艺水或母液,再启动反应釜进行搅拌,同时升温；步骤三,当反应釜内的MBT完全溶解后,向反应釜内含固率为10％补入工艺水或母液,将反应釜内温度降至40-50℃后保持温度不变；步骤四,按照醋酸铜与MBT的摩尔比为1:1200-2000称取醋酸铜的量,并将醋酸铜加入到反应釜内对MBT进行提纯。本发明的有益效果是本发明不会产生大量废水,减少水处理成本,同时在处理过程中所有水都可以回用,相比于溶剂法提纯本发明可以避免溶剂使用,更加安全。(The invention relates to the technical field of accelerators, in particular to a purification process of an accelerator MBT, which comprises the following steps: step one, weighing a certain amount of MBT and ammonia water, wherein the molar ratio of the MBT to the ammonia water is 1: 3; putting the weighed MBT and ammonia water into a reaction kettle, adding process water or mother liquor according to the solid content of 20%, starting the reaction kettle to stir, and simultaneously heating; step three, after the MBT in the reaction kettle is completely dissolved, supplementing process water or mother liquor with the solid content of 10 percent into the reaction kettle, reducing the temperature in the reaction kettle to 40-50 ℃, and keeping the temperature unchanged; step four, weighing the amount of the copper acetate according to the molar ratio of the copper acetate to the MBT of 1:1200-2000, and adding the copper acetate into the reaction kettle to purify the MBT. The invention has the advantages that the invention can not generate a large amount of waste water, reduces the water treatment cost, can recycle all water in the treatment process, can avoid the use of solvent compared with the solvent method for purifying, and is safer.)

1. The purification process of the accelerator MBT is characterized by comprising the following steps:

step one, weighing a certain amount of MBT and ammonia water, wherein the molar ratio of the MBT to the ammonia water is 1: 3;

putting the weighed MBT and ammonia water into a reaction kettle, adding process water or mother liquor according to the solid content of 20%, starting the reaction kettle to stir, and simultaneously heating;

step three, after the MBT in the reaction kettle is completely dissolved, supplementing process water or mother liquor with the solid content of 10 percent into the reaction kettle, reducing the temperature in the reaction kettle to 40-50 ℃, and keeping the temperature unchanged;

step four, weighing the amount of copper acetate according to the molar ratio of the copper acetate to the MBT of 1:1200-2000, and adding the copper acetate into the reaction kettle to purify the MBT;

step five, when the MBT solution becomes a clear transparent solution, the resin is completely separated out, and the resin is filtered to obtain a new MBT solution;

step six, distilling and filtering the MBT new solution obtained in the step five, and drying to obtain high-purity MBT;

and step seven, packaging the high-purity MBT.

2. The process for purifying accelerator MBT according to claim 1, wherein the mother liquor obtained by filtration in step six is recycled at 100%.

3. The process for purifying accelerator MBT according to claim 1, wherein in step two, the temperature is raised to 80-90 ℃.

4. The process for purifying accelerator MBT according to any one of claims 1 to 3, wherein in step four, the molar ratio of copper acetate to MBT is 1: 1600.

Technical Field

The invention relates to the technical field of accelerators, in particular to a purification process of an accelerator MBT.

Background

The existing purification process of the accelerator MBT mainly comprises an oxygen oxidation process, a solvent purification process and an acid-base method purification process, wherein the risk coefficients of the oxygen oxidation process and the solvent purification process are high, a large amount of wastewater is generated by the acid-base method, the water treatment difficulty is high, and the methods are not in accordance with the requirements of the existing safe and clean production, so that a new purification process is required to be provided to solve the problems.

Disclosure of Invention

The invention aims to provide a purification process of an accelerator MBT, which aims to solve the problems in the background technology.

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

a purification process of an accelerator MBT comprises the following steps:

step one, weighing a certain amount of MBT and ammonia water, wherein the molar ratio of the MBT to the ammonia water is 1: 3;

putting the weighed MBT and ammonia water into a reaction kettle, adding process water or mother liquor according to the solid content of 20%, starting the reaction kettle to stir, and simultaneously heating;

step three, after the MBT in the reaction kettle is completely dissolved, supplementing process water or mother liquor with the solid content of 10 percent into the reaction kettle, reducing the temperature in the reaction kettle to 40-50 ℃, and keeping the temperature unchanged;

step four, weighing the amount of copper acetate according to the molar ratio of the copper acetate to the MBT of 1:1200-2000, and adding the copper acetate into the reaction kettle to purify the MBT;

step five, when the MBT solution becomes a clear transparent solution, the resin is completely separated out, and the resin is filtered to obtain a new MBT solution;

step six, distilling and filtering the MBT new solution obtained in the step five, and drying to obtain high-purity MBT;

and step seven, packaging the high-purity MBT.

The further technical effects of the invention are as follows: and sixthly, recycling 100 percent of the mother liquor obtained by filtering.

The invention has the following further technical effects: in the second step, the temperature is raised to 80-90 ℃.

The invention has the following further technical effects: in step four, the molar ratio of copper acetate to MBT was 1: 1600.

The invention has the advantages that the invention can not generate a large amount of waste water, reduces the water treatment cost, can recycle all water in the treatment process, can avoid the use of solvent compared with the solvent method for purifying, and is safer.

Drawings

FIG. 1 is a process flow diagram of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.

A purification process of an accelerator MBT comprises the following steps:

step one, weighing a certain amount of MBT and ammonia water, wherein the molar ratio of the MBT to the ammonia water is 1: 3;

step two, putting the weighed MBT and ammonia water into a reaction kettle, adding process water or mother liquor according to the solid content of 20%, starting the reaction kettle to stir, and simultaneously heating to 80-90 ℃;

step three, after the MBT in the reaction kettle is completely dissolved, supplementing process water or mother liquor with the solid content of 10 percent into the reaction kettle, expanding a reaction system, reducing the temperature in the reaction kettle to 40-50 ℃, keeping the temperature unchanged, and preparing for oxidation;

step four, weighing the amount of copper acetate according to the molar ratio of the copper acetate to the MBT of 1:1200-2000, and adding the copper acetate into the reaction kettle to purify the MBT;

step five, when the MBT solution becomes a clear transparent solution, the resin is completely separated out, and the resin is filtered to obtain a new MBT solution;

step six, distilling and filtering the MBT new solution obtained in the step five, and drying to obtain high-purity MBT; the purity of the MBT obtained by the method reaches more than 98 percent, and the melting point is more than 175 ℃;

and step seven, packaging the high-purity MBT.

Furthermore, the mother liquor obtained by filtering in the sixth step is recycled by 100 percent, so that waste is avoided.

Furthermore, in step four, the molar ratio of copper acetate to MBT is 1:1600, and at this molar ratio, the purification effect is better.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.