阅读说明：本技术 一种废水破乳剂生产工艺 (Production process of wastewater demulsifier ) 是由 颜东峰 于 2021-07-23 设计创作，主要内容包括：本发明涉及一种废水破乳剂生产工艺,包括以下步骤：包括以下步骤：(1)在搅拌机中先放入丙烯酸,三乙醇胺和浓硫酸进行搅拌,再升温至100-120℃,保温时间0.5-1h；(2)向步骤(1)的搅拌机中分别滴加过硫酸铵和VC,滴加过程中升温速度为每分钟10℃直到搅拌机内温度为150℃,继续保温至滴加结束,得到混料；(3)将步骤(2)得到的混料放入冷凝回流容器中,边搅拌边依次加入N,N-二甲基甲酰胺和对苯二酚,冷凝回流加热后,待冷却至室温后即得到废水破乳剂。本发明采用分段加入试剂,并且配合滴加方式加入其它试剂可以使试剂之间反应更均匀,制备出的废水破乳剂的破乳效果好,且速度快,用量少且环保。(The invention relates to a production process of a wastewater demulsifier, which comprises the following steps: the method comprises the following steps: (1) firstly, acrylic acid, triethanolamine and concentrated sulfuric acid are added into a stirrer for stirring, then the temperature is increased to 120 ℃ and the heat preservation time is 0.5-1 h; (2) respectively dropwise adding ammonium persulfate and VC into the stirrer in the step (1), wherein the heating rate is 10 ℃ per minute in the dropwise adding process until the temperature in the stirrer is 150 ℃, and continuously preserving the heat until the dropwise adding is finished to obtain a mixed material; (3) and (3) putting the mixed material obtained in the step (2) into a condensation reflux container, sequentially adding N, N-dimethylformamide and hydroquinone while stirring, carrying out condensation reflux heating, and cooling to room temperature to obtain the wastewater demulsifier. According to the invention, reagents are added in sections, and other reagents are added in a dropwise manner, so that the reagents can react more uniformly, and the prepared wastewater demulsifier has the advantages of good demulsification effect, high speed, small dosage and environmental friendliness.)

1. A production process of a wastewater demulsifier is characterized by comprising the following steps: the method comprises the following steps:

(1) firstly, acrylic acid, triethanolamine and concentrated sulfuric acid are added into a stirrer for stirring, then the temperature is increased to 120 ℃ and the heat preservation time is 0.5-1 h;

(2) respectively dropwise adding ammonium persulfate and VC into the stirrer in the step (1), wherein the heating rate is 10 ℃ per minute in the dropwise adding process until the temperature in the stirrer is 150 ℃, and continuously preserving the heat until the dropwise adding is finished to obtain a mixed material;

(3) and (3) putting the mixed material obtained in the step (2) into a condensation reflux container, sequentially adding N, N-dimethylformamide and hydroquinone while stirring, carrying out condensation reflux heating, and cooling to room temperature to obtain the wastewater demulsifier.

2. The production process of the wastewater demulsifier according to claim 1, wherein the production process comprises the following steps: the stirring conditions in the step (1) are as follows: the stirring speed is 150-200r/min, and the stirring time is 5-10 min.

3. The production process of the wastewater demulsifier according to claim 1, wherein the production process comprises the following steps: the stirring conditions in the step (1) are as follows: the stirring speed is 180r/min, and the stirring time is 8 min.

4. The production process of the wastewater demulsifier according to claim 1, wherein the production process comprises the following steps: the dropping speed of the step (2) is 120-150 drops/min.

5. The production process of the wastewater demulsifier according to claim 1, wherein the production process comprises the following steps: the dropping speed of the step (2) is 140 drops/min.

6. The production process of the wastewater demulsifier according to claim 1, wherein the production process comprises the following steps: the heating temperature of the condensation reflux in the step (3) is 100-110 ℃, and the heating time of the condensation reflux is 1-2 h.

7. The production process of the wastewater demulsifier according to claim 1, wherein the production process comprises the following steps: the heating temperature of the condensation reflux in the step (3) is 105 ℃, and the heating time of the condensation reflux is 1.5 h.

8. The production process of the wastewater demulsifier according to claim 1, wherein the production process comprises the following steps: the mass volume relationship of the acrylic acid, the triethanolamine, the concentrated sulfuric acid, the ammonium persulfate, the VC, the N, N-dimethylformamide and the hydroquinone is as follows: 7-8g of 8-10g, 9-12ml, 3-5g of 1-2g of 30-40ml, and 0.4-0.7g of 3-5 ml.

9. The production process of the wastewater demulsifier according to claim 1, wherein the production process comprises the following steps: the mass volume relationship of the acrylic acid, the triethanolamine, the concentrated sulfuric acid, the ammonium persulfate, the VC, the N, N-dimethylformamide and the hydroquinone is as follows: 9g, 7.5g, 11ml, 4g, 1.5g, 35ml, 0.6 g.

10. The production process of the wastewater demulsifier according to claim 1, wherein the production process comprises the following steps: the step (3) also comprises the addition of 2-3g of octadecyl amine chloride.

Technical Field

The invention relates to the technical field of water pollution prevention and treatment and particularly relates to a production process of a wastewater demulsifier.

Background

The natural emulsifiers such as colloid, asphaltene and the like contained in the wastewater increase the demulsification difficulty, the oil-water density difference is small, the separation is difficult, the mineral oil contained in the wastewater has large density, the water quality and the water quantity change greatly, and the quality and the quantity of the water which comes from moment to moment change greatly. Due to the characteristics, the stability of the wastewater emulsion is enhanced, and the demulsification and separation of the wastewater are influenced.

Therefore, it is very important to research a production process of the wastewater demulsifier with good demulsification effect.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a production process of a wastewater demulsifier, which aims to solve the problems in the background art.

The technical scheme of the invention is realized as follows:

a production process of a wastewater demulsifier comprises the following steps:

(1) firstly, acrylic acid, triethanolamine and concentrated sulfuric acid are added into a stirrer for stirring, then the temperature is increased to 120 ℃ and the heat preservation time is 0.5-1 h;

(2) respectively dropwise adding ammonium persulfate and VC into the stirrer in the step (1), wherein the heating rate is 10 ℃ per minute in the dropwise adding process until the temperature in the stirrer is 150 ℃, and continuously preserving the heat until the dropwise adding is finished to obtain a mixed material;

(3) and (3) putting the mixed material obtained in the step (2) into a condensation reflux container, sequentially adding N, N-dimethylformamide and hydroquinone while stirring, carrying out condensation reflux heating, and cooling to room temperature to obtain the wastewater demulsifier.

Preferably, the stirring conditions in the step (1) are: the stirring speed is 150-200r/min, and the stirring time is 5-10 min.

Preferably, the stirring conditions in the step (1) are: the stirring speed is 180r/min, and the stirring time is 8 min.

Preferably, the dropping speed of the step (2) is 120-150 drops/min.

Preferably, the dropping speed of the step (2) is 140 drops/min.

Preferably, the heating temperature of the condensation reflux in the step (3) is 100-110 ℃, and the heating time of the condensation reflux is 1-2 h.

Preferably, the heating temperature of the condensation reflux in the step (3) is 105 ℃, and the heating time of the condensation reflux is 1.5 h.

Preferably, the mass volume relationship of the acrylic acid, the triethanolamine, the concentrated sulfuric acid, the ammonium persulfate, the VC, the N, N-dimethylformamide and the hydroquinone is as follows: 7-8g of 8-10g, 9-12ml, 3-5g of 1-2g of 30-40ml, and 0.4-0.7g of 3-5 ml.

Preferably, the mass volume relationship of the acrylic acid, the triethanolamine, the concentrated sulfuric acid, the ammonium persulfate, the VC, the N, N-dimethylformamide and the hydroquinone is as follows: 9g, 7.5g, 11ml, 4g, 1.5g, 35ml, 0.6 g.

Preferably, the step (3) further comprises adding 2-3g of octadecyl amine chloride.

The invention has the following beneficial effects:

according to the invention, reagents are added in sections, and other reagents are added in a dropwise manner, so that the reagents can react more uniformly, and the prepared wastewater demulsifier has the advantages of good demulsification effect, high speed, small dosage and environmental friendliness.

Detailed Description

For a more clear understanding of the technical features, objects and advantages of the present invention, reference is now made to the following detailed description of the embodiments of the present invention taken in conjunction with the accompanying drawings, which are included to illustrate and not to limit the scope of the present invention.

The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.

Example 1

A wastewater demulsifier comprises the following raw materials in parts by weight: the mass volume relationship of the acrylic acid, the triethanolamine, the concentrated sulfuric acid, the ammonium persulfate, the VC, the N, N-dimethylformamide, the hydroquinone and the octadecyl amine chloride is as follows: 8g, 9ml, 5g, 1g, 40ml, 0.4g, 3 g.

A production process of a wastewater demulsifier comprises the following steps:

(1) firstly, adding acrylic acid, triethanolamine and concentrated sulfuric acid into a stirrer for stirring at the stirring speed of 150r/min for 10 min; then heating to 100 ℃, and keeping the temperature for 1 h;

(2) respectively dropwise adding ammonium persulfate and VC into the stirrer in the step (1) at the dropping speed of 120 drops/min, heating at the speed of 10 ℃ per minute in the dropping process until the temperature in the stirrer is 150 ℃, and continuously preserving heat until the dropwise adding is finished to obtain a mixed material;

(3) and (3) putting the mixed material obtained in the step (2) into a condensation reflux container, sequentially adding N, N-dimethylformamide and hydroquinone while stirring, carrying out condensation reflux heating at the temperature of 100 ℃ for 2 hours, carrying out condensation reflux heating, and cooling to room temperature to obtain the wastewater demulsifier.

Example 2

A wastewater demulsifier comprises the following raw materials in parts by weight: the mass volume relationship of the acrylic acid, the triethanolamine, the concentrated sulfuric acid, the ammonium persulfate, the VC, the N, N-dimethylformamide, the hydroquinone and the octadecyl amine chloride is as follows: 9g, 7.5g, 11ml, 4g, 1.5g, 35ml, 0.6g, 2.5 g.

A production process of a wastewater demulsifier comprises the following steps:

(1) firstly, adding acrylic acid, triethanolamine and concentrated sulfuric acid into a stirrer for stirring at the stirring speed of 180r/min for 8 min; then the temperature is raised to 110 ℃, and the heat preservation time is 0.5 h;

(2) respectively dropwise adding ammonium persulfate and VC into the stirrer in the step (1) at the dropping speed of 140 drops/min, wherein the heating speed is 10 ℃ per minute in the dropping process until the temperature in the stirrer is 150 ℃, and continuously preserving the heat until the dropwise adding is finished to obtain a mixed material;

(3) and (3) putting the mixed material obtained in the step (2) into a condensation reflux container, sequentially adding N, N-dimethylformamide and hydroquinone while stirring, carrying out condensation reflux heating at the temperature of 105 ℃ for 1.5h, carrying out condensation reflux heating, and cooling to room temperature to obtain the wastewater demulsifier.

Example 3

A wastewater demulsifier comprises the following raw materials in parts by weight: the mass volume relationship of the acrylic acid, the triethanolamine, the concentrated sulfuric acid, the ammonium persulfate, the VC, the N, N-dimethylformamide, the hydroquinone and the octadecyl amine chloride is as follows: 10g, 7g, 12ml, 3g, 2g, 30ml, 0.7g, 2 g.

A production process of a wastewater demulsifier comprises the following steps:

(1) firstly, adding acrylic acid, triethanolamine and concentrated sulfuric acid into a stirrer for stirring at the stirring speed of 200r/min for 5 min; then heating to 120 ℃, and keeping the temperature for 0.5 h;

(2) respectively dropwise adding ammonium persulfate and VC into the stirrer in the step (1) at the dropping speed of 150 drops/min, wherein the heating speed is 10 ℃ per minute in the dropping process until the temperature in the stirrer is 150 ℃, and continuously preserving the heat until the dropwise adding is finished to obtain a mixed material;

(3) and (3) putting the mixed material obtained in the step (2) into a condensation reflux container, sequentially adding N, N-dimethylformamide and hydroquinone while stirring, carrying out condensation reflux heating at the temperature of 110 ℃ for 1h, carrying out condensation reflux heating, and cooling to room temperature to obtain the wastewater demulsifier.

Example 4

A wastewater demulsifier comprises the following raw materials in parts by weight: the mass volume relationship of the acrylic acid, the triethanolamine, the concentrated sulfuric acid, the ammonium persulfate, the VC, the N, N-dimethylformamide, the hydroquinone and the octadecyl amine chloride is as follows: 9g, 7g, 11ml, 4g, 1g, 35ml, 0.6g, 2 g.

A production process of a wastewater demulsifier comprises the following steps:

(1) firstly, adding acrylic acid, triethanolamine and concentrated sulfuric acid into a stirrer for stirring at the stirring speed of 160r/min for 9 min; then heating to 105 ℃, and keeping the temperature for 1 h;

(2) respectively dropwise adding ammonium persulfate and VC into the stirrer in the step (1) at the dropping speed of 140 drops/min, wherein the heating speed is 10 ℃ per minute in the dropping process until the temperature in the stirrer is 150 ℃, and continuously preserving the heat until the dropwise adding is finished to obtain a mixed material;

(3) and (3) putting the mixed material obtained in the step (2) into a condensation reflux container, sequentially adding N, N-dimethylformamide and hydroquinone while stirring, carrying out condensation reflux heating at the temperature of 105 ℃ for 1h, carrying out condensation reflux heating, and cooling to room temperature to obtain the wastewater demulsifier.

Comparative example 1

The waste water demulsifier prepared by the production process of the embodiment 2 of the invention has the unique difference that the stirring speed in the step (1) is 25-300 r/min, and the stirring time is 20-30 min.

Comparative example 2

The only difference of the wastewater demulsifier prepared by the production process of the embodiment 2 of the invention is that the dropping speed in the step (2) is 60-80 drops/min.

The demulsification performance of the wastewater demulsifiers prepared in examples 1 to 4 and comparative examples 1 to 3 was tested, and the test results are shown in tables 1 to 3 below.

TABLE 1 demulsification Performance of wastewater demulsifiers prepared in examples 1-3 and comparative examples 1-2

	Example 1	Example 2	Example 3	Example 4	Comparative example 1	Comparative example 2
							Transmittance (%)	91.2	92.3	91.6	88.7	34.5	33.6
Absorbance of the solution	0.556	0.543	0.564	0.543	0.611	0.634
							SedimentationPercentage (%)	89.5	88.5	87.3	88.9	44.6	45.9

The sedimentation rate of the demulsifier of the embodiments 1 to 4 of the invention can reach 91.6 percent to the maximum and is 45.9 percent higher than that of the demulsifier of the comparative example, obviously, the demulsifier of the wastewater prepared by the preparation method of the invention has better demulsification effect than that of the demulsifier of the comparative examples 1 to 2.

The above embodiments are merely provided to help understand the method and core principle of the present invention, and the main steps and embodiments of the present invention are described in detail by using specific examples. To those skilled in the art, the various conditions and parameters may be varied as desired in a particular implementation in accordance with the principles of the invention, and in view of the foregoing, the description is not to be taken as limiting the invention.