阅读说明：本技术 一种端羧基超支化物活化的锌离子除味剂的制备方法 (Preparation method of zinc ion deodorant activated by carboxyl-terminated hyperbranched compound ) 是由 杜广燎 于 2021-09-02 设计创作，主要内容包括：本发明公开了一种端羧基超支化物活化的锌离子除味剂的制备方法,具体步骤为：S1：水性超支化聚酯的合成：将三羟甲基丙烷和二羟甲基丙酸按照一定的比例加入反应器中,升温至150℃,通氮气保护,加入适量催化剂A,反应3h后减压脱去生成的水分；S2：端羧基超支化聚合物的合成：向S1步骤中的产物加入一定量的酸酐,保温150℃,反应2h后,将温度降至95℃；S3：端羧基超支化物与锌离子的皂化反应：用一定量的水将S2步骤中的产物溶解,保温在95℃,再加入一定量的锌盐或者氧化锌,继续搅拌1h,最后降至室温出料；S4：冷却后,得到端羧基超支化物活化的锌离子除味剂。本发明合成的异味清除剂对异味分子的清除效果有明显提高。(The invention discloses a preparation method of a carboxyl-terminated hyper-branched activated zinc ion deodorant, which comprises the following specific steps: s1: synthesizing aqueous hyperbranched polyester: adding trimethylolpropane and dimethylolpropionic acid into a reactor according to a certain proportion, heating to 150 ℃, introducing nitrogen for protection, adding a proper amount of catalyst A, reacting for 3 hours, and reducing pressure to remove generated water; s2: synthesis of carboxyl-terminated hyperbranched polymer: adding a certain amount of acid anhydride into the product obtained in the step S1, keeping the temperature at 150 ℃, and reducing the temperature to 95 ℃ after reacting for 2 hours; s3: saponification of carboxyl-terminated hyperbranched product and zinc ion: dissolving the product obtained in the step S2 with a certain amount of water, keeping the temperature at 95 ℃, adding a certain amount of zinc salt or zinc oxide, continuing stirring for 1h, and finally cooling to room temperature for discharging; s4: and cooling to obtain the zinc ion deodorant activated by the carboxyl-terminated hyper-branched compound. The synthesized peculiar smell scavenger obviously improves the effect of removing peculiar smell molecules.)

1. A preparation method of a carboxyl-terminated hyper-branched activated zinc ion deodorant is characterized by comprising the following steps: the method comprises the following specific steps:

s1: synthesizing aqueous hyperbranched polyester: adding trimethylolpropane and dimethylolpropionic acid into a reactor according to a certain proportion, heating to 150 ℃, introducing nitrogen for protection, adding a proper amount of catalyst A, reacting for 3 hours, and reducing pressure to remove generated water;

s2: synthesis of carboxyl-terminated hyperbranched polymer: adding a certain amount of acid anhydride into the product obtained in the step S1, keeping the temperature at 150 ℃, and reducing the temperature to 95 ℃ after reacting for 2 hours;

s3: saponification of carboxyl-terminated hyperbranched product and zinc ion: dissolving the product obtained in the step S2 with a certain amount of water, keeping the temperature at 95 ℃, adding a certain amount of zinc salt or zinc oxide, continuing stirring for 1h, and finally cooling to room temperature for discharging;

s4: after cooling, the zinc ion deodorant activated by the carboxyl-terminated hyper-branched compound is obtained, and the final realized effective concentration of the zinc ions can reach 90 percent or even higher.

2. The method for preparing carboxyl-terminated hyper-branched activated zinc ion deodorant according to claim 1, characterized in that: the mass ratio of the trimethylolpropane to the dimethylolpropionic acid is 1:5-1: 10.

3. The method for preparing carboxyl-terminated hyper-branched activated zinc ion deodorant according to claim 2, characterized in that: the mass ratio of trimethylolpropane to dimethylolpropionic acid is 1: 9.

4. the method for preparing carboxyl-terminated hyper-branched activated zinc ion deodorant according to claim 1, characterized in that: the catalyst A is one or two of p-toluenesulfonic acid, sulfamic acid, phosphoric acid and methanesulfonic acid, and the total mass of the added reactants is 1-5%.

5. The method of claim 4, wherein the zinc ion deodorant is activated by carboxyl-terminated hyper-branched compounds, and the method comprises the following steps: the catalyst A is p-toluenesulfonic acid, and the addition amount of the catalyst A is 3%.

6. The method for preparing carboxyl-terminated hyper-branched activated zinc ion deodorant according to claim 1, characterized in that: the acid anhydride is one or two of succinic anhydride, phthalic anhydride, maleic anhydride and fumaric anhydride, and the addition amount of the acid anhydride is 10-40% of the total mass.

7. The method of claim 6, wherein the zinc ion deodorant is activated by carboxyl-terminated hyper-branched compounds, and the method comprises the following steps: the anhydride is succinic anhydride, and the addition amount of the anhydride is 25%.

8. The method for preparing carboxyl-terminated hyper-branched activated zinc ion deodorant according to claim 1, characterized in that: the zinc salt is one or two of zinc sulfate, zinc acetate and zinc phosphate, and the amount of the zinc salt is the same as that of the acid anhydride.

Technical Field

The invention belongs to the technical field of indoor odor removal, and particularly relates to a preparation method of a zinc ion odor removal agent activated by carboxyl-terminated hyperbranched compounds.

Background

With the development of economic level and the improvement of technical level, people have higher and higher requirements on living environment at their sides. The air environment is one of the most important elements in the residential environment. Can breath fresh air, and has very obvious positive and positive effects on human physiology and psychology. At present, domestic industrial development has undergone extensive development and heavy development and light treatment, so that the opportunity of harmful substances and peculiar smell (oxygen-containing organic substances such as aldehyde, phenol and alcohol, sulfur compounds such as hydrogen sulfide and sulfur dioxide, nitrogen compounds such as ammonia gas and amines) which are contacted by people is greatly increased compared with the prior art, and the long-term contact of the peculiar smell substances can cause great harm to the nervous system, the respiratory system, the endocrine system, the digestive system and the like of people, thereby causing great influence on health. How to efficiently, durably, conveniently and quickly remove harmful gases frequently encountered in life and improve the living environment is a more and more concerned problem.

The common methods for removing the odor substances at present comprise a chemical method for removing the odor, a photocatalyst for removing the odor, a porous substance adsorption method and the like. The chemical method has the advantages of quick effect, good removing effect, low cost and the like, and is widely applied. Among the numerous chemical agents for removing odors, zinc ion compounds are the most important one.

Disclosure of Invention

The invention aims to provide a preparation method of a zinc ion deodorant activated by carboxyl-terminated hyper-branched compounds, aiming at solving the problems in the background technology. In order to realize the purpose, the invention adopts the technical scheme that:

a preparation method of a carboxyl-terminated hyper-branched activated zinc ion deodorant comprises the following specific steps:

s1: synthesizing aqueous hyperbranched polyester: adding trimethylolpropane and dimethylolpropionic acid into a reactor according to a certain proportion, heating to 150 ℃, introducing nitrogen for protection, adding a proper amount of catalyst A, reacting for 3 hours, and reducing pressure to remove generated water;

s2: synthesis of carboxyl-terminated hyperbranched polymer: adding a certain amount of acid anhydride into the product obtained in the step S1, keeping the temperature at 150 ℃, and reducing the temperature to 95 ℃ after reacting for 2 hours;

s3: saponification of carboxyl-terminated hyperbranched product and zinc ion: dissolving the product obtained in the step S2 with a certain amount of water, keeping the temperature at 95 ℃, adding a certain amount of zinc salt or zinc oxide, continuing stirring for 1h, and finally cooling to room temperature for discharging;

s4: after cooling, the zinc ion deodorant activated by the carboxyl-terminated hyper-branched compound is obtained, and the final realized effective concentration of the zinc ions can reach 90 percent or even higher.

Further, the mass ratio of the trimethylolpropane to the dimethylolpropionic acid is 1:5 to 1:10,

further, the ratio of the amounts of the trimethylolpropane and dimethylolpropionic acid substances is 1: 9.

further, the catalyst A is one or two of p-toluenesulfonic acid, sulfamic acid, phosphoric acid and methanesulfonic acid, and the addition amount of the catalyst A is 1-5% of the total mass of reactants.

Further, the catalyst A is p-toluenesulfonic acid, and the addition amount of the catalyst A is 3%

Further, the acid anhydride is one or two of succinic anhydride, phthalic anhydride, maleic anhydride and fumaric anhydride, and the addition amount of the acid anhydride is 10-40% of the total mass.

Further, the acid anhydride is succinic anhydride, and the addition amount of the acid anhydride is 25 percent

Further, the zinc salt is one or two of zinc sulfate, zinc acetate and zinc phosphate, and the amount of the substances is the same as that of the acid anhydride.

The invention has the beneficial effects that:

1. the hyperbranched polymer is a highly branched three-dimensional macromolecule, has a plurality of branching points, is not easy to tangle molecular chains, and has high functionality of terminal functional groups.

2. The contact sites of the carboxyl-terminated hyper-branched compound and zinc ions are more, so that the concentration of the activated zinc ions is greatly improved. Experiments prove that the peculiar smell remover synthesized by the patent has obviously improved effect of removing peculiar smell molecules;

3. the formaldehyde removal efficiency is 80 percent, the hydrogen sulfide removal efficiency is 73 percent and the ammonia gas cleaning efficiency is 90 percent within 45 min.

Drawings

Fig. 1 is a schematic diagram of a product generation process provided in an embodiment of the present invention.

Detailed Description

To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.

It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. In contrast, when an element is referred to as being "directly on" another element, there are no intervening elements present. As used herein, the terms "vertical," "horizontal," "left," "right," and the like are for illustrative purposes only and do not represent the only embodiments, and as used herein, the terms "upper," "lower," "left," "right," "front," "rear," and the like are used in a positional relationship with reference to the drawings.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

The technical solution of the present patent will be described in further detail with reference to the following embodiments.

As shown in fig. 1, the embodiment of the present invention provides a preparation method of a carboxyl-terminated hyperbranched compound activated zinc ion deodorant, which comprises the following specific steps:

s1: synthesizing aqueous hyperbranched polyester: adding trimethylolpropane and dimethylolpropionic acid into a reactor according to a certain proportion, heating to 150 ℃, introducing nitrogen for protection, adding a proper amount of catalyst A, reacting for 3 hours, and reducing pressure to remove generated water;

s2: synthesis of carboxyl-terminated hyperbranched polymer: adding a certain amount of acid anhydride into the product obtained in the step S1, keeping the temperature at 150 ℃, and reducing the temperature to 95 ℃ after reacting for 2 hours;

s3: saponification of carboxyl-terminated hyperbranched product and zinc ion: dissolving the product obtained in the step S2 with a certain amount of water, keeping the temperature at 95 ℃, adding a certain amount of zinc salt or zinc oxide, continuing stirring for 1h, and finally cooling to room temperature for discharging;

s4: after cooling, the zinc ion deodorant activated by the carboxyl-terminated hyper-branched compound is obtained, and the final realized effective concentration of the zinc ions can reach 90 percent or even higher.

In this embodiment, the amount ratio of the trimethylolpropane and dimethylolpropionic acid is 1:5 to 1:10,

in this embodiment, the ratio of the amounts of trimethylolpropane and dimethylolpropionic acid is 1: 9.

in the specific embodiment, the catalyst A is one or two of p-toluenesulfonic acid, sulfamic acid, phosphoric acid and methanesulfonic acid, and the addition amount of the catalyst A is 1-5% of the total mass of reactants.

In this embodiment, the catalyst a is p-toluenesulfonic acid, and the addition amount thereof is 3%.

In the specific embodiment, the acid anhydride is one or two of succinic anhydride, phthalic anhydride, maleic anhydride and fumaric anhydride, and the addition amount of the acid anhydride is 10-40% of the total mass.

In the specific embodiment, the acid anhydride is succinic anhydride, and the addition amount of the acid anhydride is 25 percent

In the embodiment, the zinc salt is one or two of zinc sulfate, zinc acetate and zinc phosphate, and the amount of the substance is the same as that of the acid anhydride.

The odor scavenger prepared by the embodiment is adopted to remove odor, the odor scavenger with the same amount of commercial Evonik TEGO A30 is adopted as a control group, formaldehyde, hydrogen sulfide and ammonia gas are respectively removed for experiments, and after the odor scavenger is removed for 45min, the effects are shown in the following table:

TABLE 1 Formaldehyde, hydrogen sulfide, ammonia gas scavenging effect

Item	The removal efficiency of formaldehyde%	The scavenging efficiency of hydrogen sulfide%	The removal efficiency of ammonia gas%
				Examples	80	73	90
Control group	70	70	75

As can be seen from the above table, compared with the odor scavenger of Evonik TEGO a30 sold in the market, the odor scavenger prepared in the embodiment 1 of the present invention has an excellent odor scavenging effect, wherein the formaldehyde scavenging efficiency is 80%, the hydrogen sulfide scavenging efficiency is 73%, and the ammonia scavenging efficiency is 90% within 45 min.

The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.