阅读说明：本技术 一种熔融法合成月桂酸锌的清洁生产工艺 (Clean production process for synthesizing zinc laurate by melting method ) 是由 石淑敏 周绍煌 罗芷珊 张杰鹏 胡丹 荀育军 谭志佳 周述辉 王玉梅 于 2020-05-26 设计创作，主要内容包括：本发明公开了一种熔融法合成月桂酸锌的清洁生产工艺,包括：将一定量的月桂酸投入反应釜中,升温至一定温度使月桂酸全部熔融,继续升温至80-160℃,一次性向反应釜中加入按一定配比称量好的氧化锌和催化剂,在搅拌的条件下反应一定时间得到熔融月桂酸锌,进一步的进行喷雾造粒得到颗粒状月桂酸锌。本发明合成工艺简单,不产生工业废水,产品质量高,成本低,熔融法合成月桂酸锌具有一定的环保意义,所合成的月桂酸锌具有良好的应用前景。(The invention discloses a clean production process for synthesizing zinc laurate by a melting method, which comprises the following steps: adding a certain amount of lauric acid into a reaction kettle, heating to a certain temperature to completely melt the lauric acid, continuously heating to 80-160 ℃, adding zinc oxide and a catalyst which are weighed according to a certain proportion into the reaction kettle at one time, reacting for a certain time under the condition of stirring to obtain molten zinc laurate, and further performing spray granulation to obtain granular zinc laurate. The method has the advantages of simple synthesis process, no industrial wastewater, high product quality and low cost, and the zinc laurate synthesized by the melting method has certain environmental protection significance and has good application prospect.)

1. A clean production process for synthesizing zinc laurate by a melting method is characterized by comprising the following steps: the method comprises the following steps:

step one, putting stearic acid into a reaction kettle, and heating to 60-100 ℃;

step two, after the stearic acid is completely melted, heating to 80-160 ℃, and adding zinc oxide and a catalyst once again;

filling nitrogen to make the initial pressure of the reaction kettle be 0-0.5 Mpa;

step four, further stirring and reacting for 1-5h at the temperature of 80-160 ℃ under the action of a catalyst;

and fifthly, directly conveying the molten zinc laurate to a spray granulation tower through a conveying pipeline after the reaction is finished, spraying vaporous zinc laurate through a spray head configured on the spray granulation tower, and conveying cold air upwards from the lower part at the same time to enable the vaporous zinc laurate to be fully contacted with the cold air, so that granular zinc laurate is finally obtained.

2. The clean production process for synthesizing zinc laurate according to the claim 1, which is characterized in that: and the catalyst in the second step is one or more of water, hydrogen peroxide and glacial acetic acid.

3. The clean production process for synthesizing zinc laurate according to the claim 1, which is characterized in that: and the reaction kettle in the third step is a high-pressure reaction kettle or a horizontal closed reaction kettle.

4. The clean production process for synthesizing zinc laurate according to the claim 1, which is characterized in that: step four the reaction temperature of lauric acid and zinc oxide is preferably 130-145 ℃.

5. The clean production process for synthesizing zinc laurate according to the claim 1, which is characterized in that: and step four, the lauric acid and the zinc oxide are stirred for reaction for 1.5 to 3.5 hours.

6. The clean production process for synthesizing zinc laurate according to the claim 1, which is characterized in that: when the initial pressure is 0MPa, nitrogen is not filled in to carry out the normal pressure synthesis reaction.

7. The clean production process for synthesizing zinc laurate according to the claim 1, which is characterized in that: the mass ratio of the zinc oxide to the lauric acid is as follows: 5:1-1.1.

8. The clean production process for synthesizing zinc laurate according to the claim 1, which is characterized in that: the addition amount of the catalyst is 8-15% of that of the zinc oxide.

9. The clean production process for synthesizing zinc laurate according to the claim 1, which is characterized in that: the particle size of the zinc laurate can be controlled by adjusting the spraying speed of the spray head.

10. The clean production process for synthesizing zinc laurate according to the claim 1, which is characterized in that: the humidity of the cold air is 40-60%, and the temperature is 5-15 ℃.

Technical Field

The invention relates to the technical field of synthesis of zinc laurate, in particular to a clean production process for synthesizing zinc laurate by a melting method.

Background

The molecular formula of zinc laurate is Zn [ CH3(CH2)10COO ]2, the zinc laurate is slightly soluble in water, the melting point is about 130 ℃, the zinc laurate has very good emulsifying property, dispersing property and lubricating property, and the zinc laurate is widely applied in the fields of plastics, coatings, lubricating grease, textiles, buildings, papermaking, pigments, daily chemicals and the like, but the reports on the properties of the zinc laurate and the preparation method are less.

The traditional process for producing zinc laurate is a double decomposition method, and the method has the defects of complex synthesis process, low product yield and quality, more required equipment and larger investment, and simultaneously, the double decomposition method can generate a large amount of wastewater, does not accord with the development direction of green industry advocated by the state, still needs a large amount of funds for treating the wastewater, and further increases the cost.

If the zinc laurate is synthesized by the melting method, the defects can be avoided, the green clean production process has positive social benefits, but the detailed published reports about the zinc laurate synthesized by the melting method are almost absent, so that the research on the clean production process of the zinc laurate by the melting method has important value.

Disclosure of Invention

The invention aims to solve the technical problem of providing a clean production process for synthesizing zinc laurate by a melting method, which has the advantages of simple process flow, low reaction temperature (80-160 ℃), few reaction control points, no wastewater, high yield and high quality of obtained products, and the synthesized products can be directly sprayed and granulated to obtain granular zinc laurate.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a clean production process for synthesizing zinc laurate by a melting method comprises the following steps:

step one, putting stearic acid into a reaction kettle, and heating to 60-100 ℃;

step two, after the stearic acid is completely melted, heating to 80-160 ℃, and adding zinc oxide and a catalyst once again;

filling nitrogen to make the initial pressure of the reaction kettle be 0-0.5 Mpa;

step four, further stirring and reacting for 1-5h at the temperature of 80-160 ℃ under the action of a catalyst;

and fifthly, directly conveying the molten zinc laurate to a spray granulation tower through a conveying pipeline after the reaction is finished, spraying vaporous zinc laurate through a spray head configured on the spray granulation tower, and conveying cold air upwards from the lower part at the same time to enable the vaporous zinc laurate to be fully contacted with the cold air, so that granular zinc laurate is finally obtained.

In the above technical scheme, the catalyst in the second step is one or more of water, hydrogen peroxide and glacial acetic acid.

In the above technical scheme, the reaction kettle in the third step is a high-pressure reaction kettle or a horizontal closed reaction kettle.

In the above technical solution, the reaction temperature of lauric acid and zinc oxide in the fourth step is preferably 130-145 ℃.

In the technical scheme, the lauric acid and the zinc oxide in the step four are suitably stirred for reaction for 1.5-3.5 h.

In the technical scheme, the normal pressure synthesis reaction is carried out without filling nitrogen when the initial pressure is 0 MPa.

In the above technical scheme, the mass ratio of zinc oxide to lauric acid is: 5:1-1.1.

In the technical scheme, the addition amount of the catalyst is 8-15% of that of the zinc oxide.

In the technical scheme, the particle size of the zinc laurate can be controlled by adjusting the spraying speed of the spray head.

In the technical scheme, the humidity of the cold air is 40-60%, and the temperature is 5-15 ℃.

The invention has the beneficial effects that:

1. the method adopts a melting method to synthesize the zinc laurate, has the advantages of less required equipment, simple process flow, less reaction control points, easy operation, high quality of synthesized products, no wastewater, saving of a large amount of wastewater treatment funds, cost reduction, market competitiveness increase, green and clean production process and positive social benefits.

2. The catalyst adopted by the invention is one or more of water, hydrogen peroxide and glacial acetic acid, and has low price, good catalytic effect and no influence on the aspect of impurities of the synthetic product.

3. The molten zinc laurate generated by the reaction can be directly sprayed and granulated, so that the dust pollution of a production workshop is reduced, the cost is saved, and the method has environmental protection significance.

Detailed Description

A clean production process for synthesizing zinc laurate by a melting method comprises the following steps:

step one, adding lauric acid into a reaction kettle, and heating to 60-100 ℃.

Step two, after the lauric acid is completely melted, heating to 80-160 ℃, and adding zinc oxide and a catalyst once again; the reaction temperature is 80-160 ℃, and the reaction temperature range includes any point temperature, preferably 130-150 ℃, and most preferably 145 ℃. The catalyst is as follows: one or more of water, hydrogen peroxide and glacial acetic acid. The weight ratio of lauric acid to zinc oxide is as follows: 5:1-1.1, most preferably 5: 1.05. The amount of catalyst added is 8% to 15%, most preferably 15% of the zinc oxide.

Filling nitrogen to ensure that the initial pressure of the reaction kettle is 0-0.5MPa, and carrying out non-pressurized reaction when the initial pressure of the reaction kettle is 0 MPa; the pressure in the reaction kettle is 0-0.5MPa, and the most preferable initial pressure is 0.3 MPa. The reaction kettle is a high-pressure reaction kettle or a horizontal closed reaction kettle, and the normal-pressure synthesis reaction is carried out without filling nitrogen when the initial pressure is 0 MPa.

And step four, further stirring and reacting for 1-5 hours at the temperature of 80-160 ℃ under the action of a catalyst.

And step five, directly conveying the molten zinc laurate to a spray granulation tower through a conveying pipeline after the reaction is finished, spraying vaporous zinc laurate through a spray head configured on the spray granulation tower, and conveying cold air (5-15 ℃) with higher humidity (40-60%) upwards from the lower part to enable the vaporous zinc laurate to be fully contacted with the cold air, so that granular zinc laurate is finally obtained, and the synthesized zinc laurate is white in color. The particle size of the granular zinc laurate can be changed by regulating the spraying speed of the spray head, and further, the faster the spraying speed is, the smaller the obtained particles are.

For purposes of detailed description, the following are specific examples of the invention:

example 1

Putting 500g of lauric acid into a high-pressure reaction kettle, heating to 80 ℃ to completely melt the lauric acid, heating to 145 ℃, putting 105g of zinc oxide and 16.5g of water into the high-pressure reaction kettle at one time, filling nitrogen into the high-pressure reaction kettle to enable the pressure to be 0.3MPa, further starting a stirring device, stirring and reacting for 2.5 hours at 145 ℃, conveying the molten zinc laurate to a spray granulation device, further spraying atomized zinc laurate through a spray head, and simultaneously conveying cold air with high humidity from bottom to top to obtain granular zinc laurate.

Example 2

Putting 500g of lauric acid into a high-pressure reaction kettle, heating to 80 ℃ to completely melt the lauric acid, heating to 150 ℃, putting 109g of zinc oxide and 15g of water into the high-pressure reaction kettle at one time, further starting a stirring device, stirring and reacting for 3 hours at 150 ℃, conveying the molten zinc laurate to a spray granulation device, further spraying atomized zinc laurate through a spray head, and simultaneously conveying cold air with higher humidity from bottom to top to obtain granular zinc laurate.

And (3) carrying out related index detection on the zinc laurate synthesized in the embodiment.

Parameter(s)	Example 1	Example 2
			Free acid value (%)	0.94	0.96
Zinc content (%)	14.11	13.85
			Melting Point (. degree.C.)	130.8	131.2

By comparing the above table with example 1 and example 2, it is demonstrated that under the reaction conditions of the present invention, the acid value of the finished zinc laurate is less than 1%, the content is about 14.14% of theoretical value, the melting point is 131 ℃, the overall index is relatively stable, and the above process conditions result in ideal results.

The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification of the above embodiment, such as modification of parameters and materials, and other similar changes and modifications, which do not depart from the technical spirit of the present invention, are all within the scope of the present invention.