阅读说明：本技术 一种新型咪唑啉烷基胍缓蚀杀菌剂的制备方法 (Preparation method of novel imidazoline alkylguanidine corrosion inhibition bactericide ) 是由 兰丽 高敬瑜 于 2019-11-01 设计创作，主要内容包括：一种新型咪唑啉烷基胍缓蚀杀菌剂的制备方法,其特征在于所述的新型咪唑啉烷基胍缓蚀杀菌剂的制备方法包括如下步骤：步骤(1)：在装有分水器和冷凝管的四口烧瓶中加入脂肪酸、多乙烯多胺以及携水剂,升温至130～160℃,反应3～5小时,继续升温至210～240℃,反应6～10小时,利用减压蒸馏除去多余的携水剂和未反应的多乙烯多胺,得到脂肪酸基咪唑啉；步骤(2)：将上述得到的脂肪酸基咪唑啉与盐酸胍混合,升温至150～200℃,保温2～4小时,得到一种新型咪唑啉烷基胍缓蚀杀菌剂。(A preparation method of a novel imidazoline alkylguanidine corrosion inhibition bactericide is characterized by comprising the following steps: step (1): adding fatty acid, polyethylene polyamine and a water carrying agent into a four-neck flask provided with a water separator and a condenser, heating to 130-160 ℃, reacting for 3-5 hours, continuously heating to 210-240 ℃, reacting for 6-10 hours, and removing redundant water carrying agent and unreacted polyethylene polyamine by using reduced pressure distillation to obtain fatty acid base imidazoline; step (2): mixing the obtained fatty acid-based imidazoline with guanidine hydrochloride, heating to 150-200 ℃, and preserving heat for 2-4 hours to obtain the novel imidazoline alkylguanidine corrosion inhibition bactericide.)

1. A preparation method of a novel imidazoline alkylguanidine corrosion inhibition bactericide is characterized by comprising the following steps:

step (1): adding fatty acid, polyethylene polyamine and a water carrying agent into a four-neck flask provided with a water separator and a condenser, heating to 130-160 ℃, reacting for 3-5 hours, continuously heating to 210-240 ℃, reacting for 6-10 hours, and removing redundant water carrying agent and unreacted polyethylene polyamine by using reduced pressure distillation to obtain fatty acid base imidazoline.

Step (2): mixing the obtained fatty acid-based imidazoline with guanidine hydrochloride, heating to 150-200 ℃, and preserving heat for 2-4 hours to obtain the novel imidazoline alkylguanidine corrosion inhibition bactericide.

2. The process for preparing a novel imidazolinium alkylguanidine corrosion-inhibiting biocide as claimed in claim 1, wherein: the fatty acid in the step (1) is one or a mixture of oleic acid and lauric acid.

3. The process for preparing a novel imidazolinium alkylguanidine corrosion-inhibiting biocide as claimed in claim 1, wherein: the polyethylene polyamine in the step (1) is one of diethylenetriamine or triethylenetetramine.

4. The process for preparing a novel imidazolinium alkylguanidine corrosion-inhibiting biocide as claimed in claim 1, wherein: the molar ratio of the fatty acid to the polyethylene polyamine in the step (1) is 1: 1.1-1.2.

5. The process for preparing a novel imidazolinium alkylguanidine corrosion-inhibiting biocide as claimed in claim 1, wherein: the water carrying agent in the step (1) is one of toluene or xylene.

6. The process for preparing a novel imidazolinium alkylguanidine corrosion-inhibiting biocide as claimed in claim 1, wherein: the water carrying agent accounts for 15-35% of the total reaction mass fraction in the step (1).

7. The process for preparing a novel imidazolinium alkylguanidine corrosion-inhibiting biocide as claimed in claim 1, wherein: the molar ratio of the fatty acid-based imidazoline to the guanidine hydrochloride in the step (2) is (1-2) to 1.

8. The method for preparing a novel imidazoline alkylguanidine corrosion inhibition bactericide according to claim 1, wherein the method can obtain a novel imidazoline alkylguanidine corrosion inhibition bactericide.

Technical Field

The invention belongs to the technical field of chemical corrosion prevention and sterilization, and particularly relates to a preparation method of a novel imidazoline alkylguanidine corrosion inhibition bactericide.

Background

In recent years, oil fields containing various corrosive media such as hydrogen sulfide, carbon dioxide and hypersalinity formation water are in succession in appearance to cause serious corrosion of equipment, and people are attracted high attention.

In addition, microbial corrosion caused by Sulfate Reducing Bacteria (SRB) is also prevalent, and corrosion of oilfield equipment not only causes huge economic loss to development and production of the oilfield. Meanwhile, the corrosion inhibition bactericide directly threatens the living environment and physical and psychological health of human beings, and is suitable for oil field water, and needs to be developed urgently.

The largest dosage of various organic corrosion inhibitors used in the society at present is imidazoline corrosion inhibitors and derivatives thereof. Imidazoline corrosion inhibitor is a nitrogenous five-membered heterocyclic compound, is an organic corrosion inhibitor widely applied to petroleum and natural gas production, has good inhibition effect on corrosion of CO2, H2S and the like, but in consideration of corrosion problem in refining process, the chemical agent is required to be low in sulfur and preferably not sulfur.

Therefore, the development of a preparation method of the novel imidazoline alkylguanidine corrosion inhibition bactericide has necessary practical significance.

Disclosure of Invention

The invention aims to provide a preparation method of a novel imidazoline alkylguanidine corrosion inhibition bactericide, which aims to solve the problems in the background technology.

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

a preparation method of a novel imidazoline alkylguanidine corrosion inhibition bactericide is characterized by comprising the following steps:

step (1): adding fatty acid, polyethylene polyamine and a water carrying agent into a four-neck flask provided with a water separator and a condenser, heating to 130-160 ℃, reacting for 3-5 hours, continuously heating to 210-240 ℃, reacting for 6-10 hours, and removing redundant water carrying agent and unreacted polyethylene polyamine by using reduced pressure distillation to obtain fatty acid base imidazoline.

Step (2): mixing the obtained fatty acid-based imidazoline with guanidine hydrochloride, heating to 150-200 ℃, and preserving heat for 2-4 hours to obtain the novel imidazoline alkylguanidine corrosion inhibition bactericide.

Preferably, the fatty acid in the step (1) is one or a mixture of two of oleic acid and lauric acid.

Preferably, the polyethylene polyamine in the step (1) is one of diethylenetriamine and triethylenetetramine.

Preferably, the molar ratio of the fatty acid to the polyethylene polyamine in the step (1) is 1: 1.1-1.2.

Preferably, the water carrying agent in the step (1) is one of toluene or xylene.

Preferably, the water carrying agent in the step (1) accounts for 15-35% of the total reaction mass fraction.

Preferably, the molar ratio of the fatty acid-based imidazoline to the guanidine hydrochloride in the step (2) is (1-2): 1.

Preferably, the preparation method of any one of the preparation methods of the novel imidazoline alkylguanidine corrosion inhibition bactericide can obtain the novel imidazoline alkylguanidine corrosion inhibition bactericide.

The preparation method of the novel imidazoline alkylguanidine corrosion inhibition bactericide has the following beneficial effects:

at present, imidazoline corrosion inhibitors are a hotspot of corrosion inhibitor research and development, and have the advantages of good corrosion inhibition effect, small using amount, simple preparation, low toxicity, small environmental pollution, certain bactericidal performance and the like. The organic guanidine bactericide has high-efficiency broad-spectrum bactericidal performance, no toxic or side effect and environmental friendliness, and is widely applied to medicines, plant protection, industrial products and daily necessities.

The invention provides a preparation method of a novel imidazoline alkylguanidine corrosion inhibition bactericide, aiming at overcoming the defects of the existing corrosion inhibition bactericide and effectively combining imidazoline and guanidine.

The preparation method of the novel imidazoline alkylguanidine corrosion inhibition bactericide provided by the invention has the advantages of simple preparation, safety and no toxicity, and the novel imidazoline alkylguanidine corrosion inhibition bactericide prepared according to the provided preparation method has the characteristics of good corrosion inhibition performance and excellent sterilization performance.

The performance evaluation result of the corrosion inhibition bactericide in the preparation method of the novel imidazoline alkylguanidine corrosion inhibition bactericide provided by the invention is as follows:

drawings

The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.

Fig. 1-2 are equations of the synthetic reaction of the fatty acid and diethylenetriamine in the novel imidazoline alkylguanidine corrosion inhibition bactericide provided by the invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the reaction equations 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 preparation method of a novel imidazoline alkylguanidine corrosion inhibition bactericide is characterized by comprising the following steps:

step (1): adding fatty acid, polyethylene polyamine and a water carrying agent into a four-neck flask provided with a water separator and a condenser, heating to 130-160 ℃, reacting for 3-5 hours, continuously heating to 210-240 ℃, reacting for 6-10 hours, and removing redundant water carrying agent and unreacted polyethylene polyamine by using reduced pressure distillation to obtain fatty acid base imidazoline.

Step (2): mixing the obtained fatty acid-based imidazoline with guanidine hydrochloride, heating to 150-200 ℃, and preserving heat for 2-4 hours to obtain the novel imidazoline alkylguanidine corrosion inhibition bactericide.

In the present invention, preferably, the fatty acid in the step (1) is one or a mixture of two of oleic acid and lauric acid.

In the present invention, preferably, the polyethylene polyamine in the step (1) is one of diethylenetriamine and triethylenetetramine.

In the present invention, it is preferable that the molar ratio of the fatty acid to the polyethylene polyamine in the step (1) is 1:1.1 to 1.2.

In the present invention, preferably, the water carrying agent in step (1) is one of toluene and xylene.

According to the invention, preferably, the water carrying agent in the step (1) accounts for 15-35% of the total reaction mass fraction.

In the present invention, the molar ratio of the fatty acid-based imidazoline to the guanidine hydrochloride in the step (2) is preferably (1-2): 1.

According to the invention, preferably, the preparation method of any one of the preparation methods of the novel imidazoline alkylguanidine corrosion inhibition bactericide can obtain the novel imidazoline alkylguanidine corrosion inhibition bactericide.

The invention relates to a preparation method of a novel imidazoline alkylguanidine corrosion inhibition bactericide, which comprises the following two steps: (1) adding fatty acid, polyethylene polyamine and a water carrying agent into a four-neck flask provided with a water separator and a condenser, heating to 130-160 ℃, reacting for 3-5 hours, continuously heating to 210-240 ℃, reacting for 6-10 hours, and removing redundant water carrying agent and unreacted polyethylene polyamine by using reduced pressure distillation to obtain fatty acid base imidazoline. Wherein, the fatty acid is one or two of oleic acid and lauric acid. The polyethylene polyamine is one of diethylenetriamine and triethylene tetramine. The molar ratio of the fatty acid to the polyethylene polyamine is 1 (1.1-1.2). The water carrying agent is one of methylbenzene and dimethylbenzene. The water carrying agent accounts for 15-35% of the total reaction mass fraction. (2) Mixing the obtained fatty acid-based imidazoline with guanidine hydrochloride, heating to 150-200 ℃, and preserving heat for 2-4 hours to obtain the novel imidazoline alkylguanidine corrosion inhibition bactericide. Wherein the molar ratio of imidazoline to guanidine hydrochloride is (1-2): 1

The invention, preferably, example 1:

(1) 169.48g of oleic acid, 68.09g of diethylenetriamine and 71.27g of xylene are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a water separator, an electric heating sleeve is heated to 150 ℃, the reaction lasts for 5 hours until no water is carried out, the water separator is changed into a distillation device, the temperature is raised to 220 ℃, the reaction lasts for 7 hours until no water is evaporated, and the pressure reduction distillation lasts for 0.5 hour to remove the redundant water-carrying agent and the unreacted diethylenetriamine, so that the oleic imidazoline I is obtained.

(2) 104.89g of oleic imidazoline and 28.66g of guanidine hydrochloride obtained in the step are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a distillation device, the temperature is raised to 180 ℃, gas is generated, diluted hydrochloric acid absorbs tail gas, the reaction is stopped for 5 hours until no gas is generated, and the novel imidazoline alkylguanidine corrosion inhibition bactericide A is obtained.

The invention, preferably, example 2:

(1) 169.48g of oleic acid, 68.09g of diethylenetriamine and 71.27g of xylene are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a water separator, an electric heating sleeve is heated to 150 ℃, the reaction lasts for 5 hours until no water is carried out, the water separator is changed into a distillation device, the temperature is raised to 220 ℃, the reaction lasts for 7 hours until no water is evaporated, and the pressure reduction distillation lasts for 0.5 hour to remove the redundant water-carrying agent and the unreacted diethylenetriamine, so that the oleic imidazoline I is obtained.

(2) 104.89g of oleic imidazoline and 19.11g of guanidine hydrochloride obtained in the step are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a distillation device, the temperature is raised to 190 ℃, gas is generated, diluted hydrochloric acid absorbs tail gas, the reaction is stopped for 6 hours until no gas is generated, and the novel imidazoline alkylguanidine corrosion inhibition bactericide B is obtained.

The invention, preferably, example 3:

(1) 169.48g of oleic acid, 68.09g of diethylenetriamine and 71.27g of xylene are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a water separator, an electric heating sleeve is heated to 150 ℃, the reaction lasts for 5 hours until no water is carried out, the water separator is changed into a distillation device, the temperature is raised to 220 ℃, the reaction lasts for 7 hours until no water is evaporated, and the pressure reduction distillation lasts for 0.5 hour to remove the redundant water-carrying agent and the unreacted diethylenetriamine, so that the oleic imidazoline I is obtained.

(2) 104.89g of oleic imidazoline and 14.33g of guanidine hydrochloride which are obtained in the above steps are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a distillation device, the temperature is raised to 200 ℃, gas is generated, diluted hydrochloric acid absorbs tail gas, the reaction is stopped for 8 hours until no gas is generated, and the novel imidazoline alkylguanidine corrosion inhibition bactericide C is obtained.

The invention, preferably, example 4:

(1) adding 120.19g of lauric acid, 105.29g of triethylene tetramine and 67.42g of xylene into a four-neck flask provided with a mechanical stirrer, a thermometer and a water separator, heating to 155 ℃ by an electric heating sleeve, reacting for 4 hours until no water is taken out, changing the water separator into a distillation device, heating to 230 ℃, reacting for 8 hours until no water is evaporated, and distilling under reduced pressure for 0.5 hour to remove redundant water carrying agent and unreacted triethylene tetramine to obtain lauroyl imidazoline I.

(2) 93.17g of lauroyl imidazoline A and 28.66g of guanidine hydrochloride which are obtained in the previous step are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a distillation device, the temperature is raised to 170 ℃, gas is generated, diluted hydrochloric acid absorbs tail gas, the reaction is stopped for 4 hours until no gas is generated, and the novel imidazoline alkylguanidine corrosion inhibition bactericide D is obtained.

The invention, preferably, example 5:

(1) adding 120.19g of lauric acid, 105.29g of triethylene tetramine and 67.42g of xylene into a four-neck flask provided with a mechanical stirrer, a thermometer and a water separator, heating to 155 ℃ by an electric heating sleeve, reacting for 4 hours until no water is taken out, changing the water separator into a distillation device, heating to 230 ℃, reacting for 8 hours until no water is evaporated, and distilling under reduced pressure for 0.5 hour to remove redundant water carrying agent and unreacted triethylene tetramine to obtain lauroyl imidazoline I.

(2) 93.17g of lauroyl imidazoline A and 19.11g of guanidine hydrochloride obtained in the step are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a distillation device, the temperature is raised to 190 ℃, gas is generated, diluted hydrochloric acid absorbs tail gas, the reaction is stopped for 6 hours until no gas is generated, and the novel imidazoline alkylguanidine corrosion inhibition bactericide E is obtained.

The invention, preferably, example 6:

(1) adding 120.19g of lauric acid, 105.29g of triethylene tetramine and 67.42g of xylene into a four-neck flask provided with a mechanical stirrer, a thermometer and a water separator, heating to 155 ℃ by an electric heating sleeve, reacting for 4 hours until no water is taken out, changing the water separator into a distillation device, heating to 230 ℃, reacting for 8 hours until no water is evaporated, and distilling under reduced pressure for 0.5 hour to remove redundant water carrying agent and unreacted triethylene tetramine to obtain lauroyl imidazoline I.

(2) 93.17g of lauroyl imidazoline A and 14.33g of guanidine hydrochloride which are obtained in the previous step are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a distillation device, the temperature is raised to 190 ℃, gas is generated, diluted hydrochloric acid absorbs tail gas, the reaction is stopped for 8 hours until no gas is generated, and the novel imidazoline alkylguanidine corrosion inhibition bactericide F is obtained.

The invention, preferably, example 7:

(1) 169.48g of oleic acid, 96.51g of triethylene tetramine and 79.80g of xylene are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a water separator, an electric heating sleeve is heated to 150 ℃, the reaction lasts for 4 hours until no water is carried out, the water separator is changed into a distillation device, the heating is carried out to 215 ℃, the reaction lasts for 5 hours until no water is evaporated, and the pressure reduction distillation lasts for 0.5 hour to remove the redundant water carrying agent and the unreacted triethylene tetramine, so that the lauroyl imidazoline II is obtained.

(2) Adding lauroyl imidazoline B157.08g and guanidine hydrochloride 38.21G obtained in the step into a four-neck flask provided with a mechanical stirrer, a thermometer and a distillation device, heating to 180 ℃, generating gas, absorbing tail gas by dilute hydrochloric acid, reacting for 5 hours until no gas is generated, and stopping the reaction to obtain the novel imidazoline alkylguanidine corrosion inhibition bactericide G.

The invention, preferably, example 8:

(1) 169.48g of oleic acid, 96.51g of triethylene tetramine and 79.80g of xylene are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a water separator, an electric heating sleeve is heated to 150 ℃, the reaction lasts for 4 hours until no water is carried out, the water separator is changed into a distillation device, the heating is carried out to 215 ℃, the reaction lasts for 5 hours until no water is evaporated, and the pressure reduction distillation lasts for 0.5 hour to remove the redundant water carrying agent and the unreacted triethylene tetramine, so that the lauroyl imidazoline II is obtained.

(2) Adding lauroyl imidazoline B157.08g and guanidine hydrochloride 25.47g obtained in the step into a four-neck flask provided with a mechanical stirrer, a thermometer and a distillation device, heating to 180 ℃, generating gas, absorbing tail gas by dilute hydrochloric acid, reacting for 8 hours until no gas is generated, and stopping the reaction to obtain the novel imidazoline alkylguanidine corrosion inhibition bactericide H.

The invention, preferably, example 9:

(1) 169.48g of oleic acid, 96.51g of triethylene tetramine and 79.80g of xylene are added into a four-neck flask provided with a mechanical stirrer, a thermometer and a water separator, an electric heating sleeve is heated to 150 ℃, the reaction lasts for 4 hours until no water is carried out, the water separator is changed into a distillation device, the heating is carried out to 215 ℃, the reaction lasts for 5 hours until no water is evaporated, and the pressure reduction distillation lasts for 0.5 hour to remove the redundant water carrying agent and the unreacted triethylene tetramine, so that the lauroyl imidazoline II is obtained.

(2) Adding lauroyl imidazoline B157.08g and guanidine hydrochloride 19.10g obtained in the step into a four-neck flask provided with a mechanical stirrer, a thermometer and a distillation device, heating to 200 ℃, generating gas, absorbing tail gas by dilute hydrochloric acid, reacting for 9 hours until no gas is generated, and stopping the reaction to obtain the novel imidazoline alkylguanidine corrosion inhibition bactericide I.

The invention, preferred, example 10:

the sewage adopted by an oil field in Jilin province is taken as a treatment object, an A3 carbon steel test piece is selected, and a dynamic corrosion evaluation test is carried out in an alloy steel kettle. Wherein the experimental dosing concentration is as follows: 70 mg/L; the temperature is as follows: 90 ℃; the partial pressure of CO2 was: 0.8 Mpa; the total pressure is: 2.0 Mpa; the rotating speed is as follows: 400 r/min; the time is as follows: and 72 h. And (4) evaluating the sterilization performance of the sulfate reducing bacteria of the water sample subjected to corrosion evaluation by adopting a bacteria bottle sterilization dilution method. The results of corrosion inhibition and sterilization evaluation are shown in Table 1, and the corrosion inhibition rate of the novel imidazoline alkylguanidine corrosion inhibition bactericide is more than or equal to 92%, and the sterilization rate is more than or equal to 99.9%.

According to the working and reaction principle of the invention, the synthesis reaction equation of the polyethylene polyamine, which is exemplified by diethylenetriamine, is as follows:

although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.