CN101643642B - High-temperature acidifying inhibiter and preparation method thereof - Google Patents
High-temperature acidifying inhibiter and preparation method thereof Download PDFInfo
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- CN101643642B CN101643642B CN2009100182206A CN200910018220A CN101643642B CN 101643642 B CN101643642 B CN 101643642B CN 2009100182206 A CN2009100182206 A CN 2009100182206A CN 200910018220 A CN200910018220 A CN 200910018220A CN 101643642 B CN101643642 B CN 101643642B
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Abstract
The invention relates to a high-temperature acidifying inhibiter and a preparation method thereof. The high-temperature acidifying inhibiter comprises the following materials in parts by weight: 79.33-87.68 of ethanol, 19-21 of methanoic acid, 22.33-24.68 of aniline, 31.11-34.39 of acetophenone, 26.13-28.88 of methanal, 31.54-34.86 of benzyl chloride and 8.55-9.45 of propiolic alcohol, wherein the ethanol, the methanoic acid and the aniline are placed into a reaction kettle to be stirred; then the acetophenone is added into the reaction kettle; then a methanal solution is dripped into the reaction kettle; the benzyl chloride is added into the reaction kettle after the methanal solution is dripped into the reaction kettle; the temperature of the reaction kettle is reduced to room temperature, and then the propiolic alcohol is added into the reaction kettle to be stirred. The water content inside the reaction kettle is low without adding an aqueous hydrochloric acid solution so as to prevent the benzyl chloride from hydrolyzing and be beneficial to reducing the unit consumption of the benzyl chloride in the quaterisation reaction process; before the methanal is completely dripped, the amount of the methanal dripped into the reaction kettle is less than the reaction mole ratio of synthetic Mannich base, the methanal is in an insufficient state so as to reduce the volatilization of the methanal, ensure the health of operators and be safer.
Description
Technical field
The present invention relates to a kind of high-temperature acidification corrosion inhibitor and preparation method thereof, belong to the oilfield chemical technical field.
Background technology
In the construction of oil field, fracture acidizing is a very important oil output measure, and almost each producing well all will pass through this one procedure; Acidizing reagent commonly used is 20% a hydrochloric acid or by hydrochloric acid and the composite mud acid that forms of hydrofluoric acid; These two kinds of acid all are acid very strong mineral acids, will cause the corrosion of down-hole string and hardware like this, and along with the increase of well depth; Temperature raises; This just will inevitably cause corrosion more serious, in order to prevent or to reduce acid solution at high temperature to the corrosion of down-hole string, will in acid solution, add high-temperature corrosion inhibitor.
At present; Acidification corrosion inhibitor commonly used mainly comprises three types of components: Mannich base, alkynol and quaternary amine; Wherein Mannich base is mainly formed by aniline, formaldehyde and methyl phenyl ketone condensation; The mode of aniline, formaldehyde and methyl phenyl ketone synthesizing mannich alkali is common building-up reactions, and promptly aniline, formaldehyde and methyl phenyl ketone are placed in the container once synthetic.
In reaction process,, just cause the volatilization of formaldehyde inevitably because formaldehyde is in the state of capacity; One ton of inhibiter of common every production, the consumption of formaldehyde is about 0.1255 ton, and consumption is bigger; Production cost is high; And, evaporateing into airborne formaldehyde operator's health has been caused great infringement, production process is dangerous.
In process of production, also need in reaction kettle, add Benzyl Chloride and aqueous hydrochloric acid, cause the interior moisture content of reaction kettle than higher; Benzyl Chloride will hydrolytic reactions; Increased the unit consumption of Benzyl Chloride in the quaternary ammonium reaction process, reduced the yield of entire reaction, one ton of inhibiter of common every production; Need to consume about 0.2066 ton Benzyl Chloride, production cost is high.
Summary of the invention
Technical problem to be solved by this invention is the problem to above-mentioned existence, and a kind of high-temperature acidification corrosion inhibitor and preparation method thereof is provided.Adopt this method to produce acidification corrosion inhibitor, production cost is low, production process safety, and the acidification corrosion inhibitor of being produced can reach the requirement of industry standard.
For solving the problems of the technologies described above, the technical scheme that the present invention adopted is: a kind of high-temperature acidification corrosion inhibitor is characterized in that: said inhibiter comprises the starting material of following parts by weight:
Ethanol 79.33-87.68 part, formic acid 19-21 part, aniline 22.33-24.68 part, methyl phenyl ketone 31.11-34.39 part, formaldehyde 26.13-28.88 part, Benzyl Chloride 31.54-34.86 part and propiolic alcohol 8.55-9.45 part.
A kind of concrete prioritization scheme, said inhibiter comprises the starting material of following parts by weight:
9 parts of 83.5 parts of ethanol, 20 parts in formic acid, 23.5 parts of aniline, 32.75 parts of methyl phenyl ketones, 27.5 parts in formaldehyde, 33.2 parts of Benzyl Chlorides and propiolic alcohols.
A kind of concrete prioritization scheme, said inhibiter comprises the starting material of following parts by weight:
8.55 parts of 79.33 parts of ethanol, 19 parts in formic acid, 22.33 parts of aniline, 31.11 parts of methyl phenyl ketones, 26.13 parts in formaldehyde, 31.54 parts of Benzyl Chlorides and propiolic alcohols.
A kind of concrete prioritization scheme, said inhibiter comprises the starting material of following parts by weight:
9.45 parts of 87.68 parts of ethanol, 21 parts in formic acid, 24.68 parts of aniline, 34.39 parts of methyl phenyl ketones, 28.88 parts in formaldehyde, 34.86 parts of Benzyl Chlorides and propiolic alcohols.
The preparation of high-temperature acidification corrosion inhibitor may further comprise the steps:
1) be ready to starting material by weight, it is 30% the aqueous solution that formaldehyde is mixed with concentration;
2) ethanol, formic acid and aniline are placed in the reaction kettle, stirred 8-18 minute;
3) methyl phenyl ketone is added in the reaction kettle, the temperature of reaction kettle is raised to 80-82 ℃, in reaction kettle, drip formaldehyde solution again, the dropping time is 20-40 minute;
4) drip formaldehyde solution after, the temperature of reaction kettle is controlled at 76.5-80.5 ℃, the time is 3-4 hour;
5) Benzyl Chloride is added in the reaction kettle, the temperature of reaction kettle is controlled at 76.5-80.5 ℃, the time is 0.5-1.5 hour;
6) temperature of reaction kettle is reduced to room temperature, add propiolic alcohol again and stirred 8-18 minute, obtain high-temperature acidification corrosion inhibitor.
The present invention adopts above technical scheme, compared with prior art, has the following advantages:
1) because need not add conventional aqueous hydrochloric acid, the moisture content in the reaction kettle is low, thereby has avoided the hydrolysis of Benzyl Chloride, helps reducing the unit consumption of Benzyl Chloride in the quaternary ammonium reaction process, improves the yield of entire reaction.The unit consumption of Benzyl Chloride is about 0.1400 ton/ton, and the Benzyl Chloride with traditional mode of production savings in comparison about 32% has reduced production cost.
2) change synthetic mode of traditional Mannich base into stepwise synthesis, taked to drip the way of formaldehyde simultaneously, following benefit is arranged like this:
A, avoid self condensation of formaldehyde, helped improving the rate of utilization of formaldehyde.
The mode that b, employing drip is added formaldehyde; Before dripping formaldehyde, be added dropwise to the reaction mol ratio that the interior formaldehyde amount of reaction kettle will be lower than synthesizing mannich alkali, formaldehyde is in state in shortage; Reduced the volatilization of formaldehyde; Thereby reduced the usage quantity of formaldehyde, guaranteed operator's health, production process is safer.The unit consumption of formaldehyde is about 0.1203 ton/ton, with the formaldehyde of traditional mode of production savings in comparison about 4.2%, has reduced the total cost of production of acidification corrosion inhibitor.
Below in conjunction with embodiment technical scheme of the present invention is further described:
Embodiment
Embodiment 1, gets the starting material of following parts by weight and produces high-temperature acidification corrosion inhibitor, 8.55 parts of 79.33 parts of ethanol, 19 parts in formic acid, 22.33 parts of aniline, 31.11 parts of methyl phenyl ketones, 26.13 parts in formaldehyde, 31.54 parts of Benzyl Chlorides and propiolic alcohols.
Produce according to following process step:
1) be ready to starting material by weight, it is 30% the aqueous solution that formaldehyde is mixed with concentration;
2) ethanol, formic acid and aniline are placed in the reaction kettle, stirred 8 minutes;
3) methyl phenyl ketone is added in the reaction kettle, the temperature of reaction kettle is raised to 80 ℃, in reaction kettle, drip formaldehyde solution again, the dropping time is 20 minutes;
4) drip formaldehyde solution after, the temperature of reaction kettle is controlled at 80 ± 0.5 ℃, the time is 3 hours;
5) Benzyl Chloride is added in the reaction kettle, the temperature of reaction kettle is controlled at 80 ± 0.5 ℃, the time is 0.5 hour;
6) temperature of reaction kettle is reduced to room temperature, add propiolic alcohol again and stirred 8 minutes, obtain high-temperature acidification corrosion inhibitor.
Use N
80The steel disc lacing film compares experiment to inhibiter in the embodiment of the invention 1 and present commercially available inhibiter; It is following to obtain the result; It is the inhibiter of HW-10S acidifying inhibition that wherein commercially available inhibiter adopts the model of Huantai County's Bimodalization plant produced, and two kinds of inhibiter all are diluted to concentration 1%.
Experimental result:
Embodiment 2, get the starting material of following parts by weight and produce high-temperature acidification corrosion inhibitor, 9 parts of 83.5 parts of ethanol, 20 parts in formic acid, 23.5 parts of aniline, 32.75 parts of methyl phenyl ketones, 27.5 parts in formaldehyde, 33.2 parts of Benzyl Chlorides and propiolic alcohols.
Produce according to following process step:
1) be ready to starting material by weight, it is 30% the aqueous solution that formaldehyde is mixed with concentration;
2) ethanol, formic acid and aniline are placed in the reaction kettle, stirred 12 minutes;
3) methyl phenyl ketone is added in the reaction kettle, the temperature of reaction kettle is raised to 81 ℃, in reaction kettle, drip formaldehyde again, the dropping time is 30 minutes;
4) drip formaldehyde after, the temperature of reaction kettle is controlled at 78 ± 0.5 ℃, the time is 4 hours;
5) Benzyl Chloride is added in the reaction kettle, the temperature of reaction kettle is controlled at 78 ± 0.5 ℃, the time is 1 hour;
6) temperature of reaction kettle is reduced to room temperature, add propiolic alcohol again and stirred 12 minutes, obtain high-temperature acidification corrosion inhibitor.
Use N
80The steel disc lacing film compares experiment to inhibiter in the embodiment of the invention 1 and present commercially available inhibiter; It is following to obtain the result; It is the inhibiter of HW-10S acidifying inhibition that wherein commercially available inhibiter adopts the model of Huantai County's Bimodalization plant produced, and two kinds of inhibiter all are diluted to concentration 1%.
Experimental result:
Embodiment 3, get the starting material of following parts by weight and produce high-temperature acidification corrosion inhibitor: 9.45 parts of 87.68 parts of ethanol, 21 parts in formic acid, 24.68 parts of aniline, 34.39 parts of methyl phenyl ketones, 28.88 parts in formaldehyde, 34.86 parts of Benzyl Chlorides and propiolic alcohols.
Produce according to following process step:
1) be ready to starting material by weight, it is 30% the aqueous solution that formaldehyde is mixed with concentration;
2) ethanol, formic acid and aniline are placed in the reaction kettle, stirred 18 minutes;
3) methyl phenyl ketone is added in the reaction kettle, the temperature of reaction kettle is raised to 82 ℃, in reaction kettle, drip formaldehyde solution again, the dropping time is 40 minutes;
4) drip formaldehyde solution after, the temperature of reaction kettle is controlled at 77 ± 0.5 ℃, the time is 5 hours;
5) Benzyl Chloride is added in the reaction kettle, the temperature of reaction kettle is controlled at 77 ± 0.5 ℃, the time is 1.5 hours;
6) temperature of reaction kettle is reduced to room temperature, add propiolic alcohol again and stirred 18 minutes, obtain high-temperature acidification corrosion inhibitor.
Use N
80The steel disc lacing film compares experiment to inhibiter in the embodiment of the invention 1 and present commercially available inhibiter; It is following to obtain the result; It is the inhibiter of HW-10S acidifying inhibition that wherein commercially available inhibiter adopts the model of Huantai County's Bimodalization plant produced, and two kinds of inhibiter all are diluted to concentration 1%.
Experimental result:
Can find out from above three embodiment, under 90 ℃ of conditions, use the resulting inhibiter of preparation method of the present invention N
80The inhibition speed index of steel disc lacing film can reach the index of the oil and gas industry SY/T 5405-1996 of the People's Republic of China standard, under 120 ℃ of conditions, to N
80The inhibition speed index of steel disc lacing film surpasses the inhibition speed index of present commercially available inhibiter.
Learn through measuring; Process using formic acid of the present invention is made catalyzer, has avoided the hydrolysis of Benzyl Chloride, and the ton unit consumption that can make Benzyl Chloride is reduced to about present 0.1400 ton/ton by original about 0.2066 ton/ton; So just make one ton of inhibiter of every production can save about 32% Benzyl Chloride; The unit consumption that can make formaldehyde is reduced to about 0.1203 ton/ton by original 0.1255 ton/ton, can make one ton of inhibiter of every production save 4.2% formaldehyde, has reduced the total cost of production of acidification corrosion inhibitor.
Claims (5)
1. high-temperature acidification corrosion inhibitor, it is characterized in that: said inhibiter is formed by the raw material preparing that comprises following parts by weight:
Ethanol 79.33-87.68 part, formic acid 19-21 part, aniline 22.33-24.68 part, methyl phenyl ketone 31.11-34.39 part, formaldehyde 26.13-28.88 part, Benzyl Chloride 31.54-34.86 part and propiolic alcohol 8.55-9.45 part;
Said preparation method may further comprise the steps:
1) be ready to starting material by weight, it is 30% the aqueous solution that formaldehyde is mixed with concentration;
2) ethanol, formic acid and aniline are placed in the reaction kettle, stirred 8-18 minute;
3) methyl phenyl ketone is added in the reaction kettle, the temperature of reaction kettle is raised to 80-82 ℃, in reaction kettle, drip formaldehyde solution again, the dropping time is 20-40 minute;
4) drip formaldehyde solution after, the temperature of reaction kettle is controlled at 76.5-80.5 ℃, the time is 3-4 hour;
5) Benzyl Chloride is added in the reaction kettle, the temperature of reaction kettle is controlled at 76.5-80.5 ℃, the time is 0.5-1.5 hour;
6) temperature of reaction kettle is reduced to room temperature, add propiolic alcohol again and stirred 8-18 minute, obtain high-temperature acidification corrosion inhibitor.
2. a kind of high-temperature acidification corrosion inhibitor as claimed in claim 1 is characterized in that: said inhibiter comprises the starting material of following parts by weight:
9 parts of 83.5 parts of ethanol, 20 parts in formic acid, 23.5 parts of aniline, 32.75 parts of methyl phenyl ketones, 27.5 parts in formaldehyde, 33.2 parts of Benzyl Chlorides and propiolic alcohols.
3. a kind of high-temperature acidification corrosion inhibitor as claimed in claim 1 is characterized in that: said inhibiter comprises the starting material of following parts by weight:
8.55 parts of 79.33 parts of ethanol, 19 parts in formic acid, 22.33 parts of aniline, 31.11 parts of methyl phenyl ketones, 26.13 parts in formaldehyde, 31.54 parts of Benzyl Chlorides and propiolic alcohols.
4. a kind of high-temperature acidification corrosion inhibitor as claimed in claim 1 is characterized in that: said inhibiter comprises the starting material of following parts by weight:
9.45 parts of 87.68 parts of ethanol, 21 parts in formic acid, 24.68 parts of aniline, 34.39 parts of methyl phenyl ketones, 28.88 parts in formaldehyde, 34.86 parts of Benzyl Chlorides and propiolic alcohols.
5. method for preparing like any described high-temperature acidification corrosion inhibitor among the claim 1-4, it is characterized in that: said preparation method may further comprise the steps:
1) be ready to starting material by weight, it is 30% the aqueous solution that formaldehyde is mixed with concentration;
2) ethanol, formic acid and aniline are placed in the reaction kettle, stirred 8-18 minute;
3) methyl phenyl ketone is added in the reaction kettle, the temperature of reaction kettle is raised to 80-82 ℃, in reaction kettle, drip formaldehyde solution again, the dropping time is 20-40 minute;
4) drip formaldehyde solution after, the temperature of reaction kettle is controlled at 76.5-80.5 ℃, the time is 3-4 hour;
5) Benzyl Chloride is added in the reaction kettle, the temperature of reaction kettle is controlled at 76.5-80.5 ℃, the time is 0.5-1.5 hour;
6) temperature of reaction kettle is reduced to room temperature, add propiolic alcohol again and stirred 8-18 minute, obtain high-temperature acidification corrosion inhibitor.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100182206A CN101643642B (en) | 2009-08-31 | 2009-08-31 | High-temperature acidifying inhibiter and preparation method thereof |
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| CN2009100182206A CN101643642B (en) | 2009-08-31 | 2009-08-31 | High-temperature acidifying inhibiter and preparation method thereof |
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| CN101643642B true CN101643642B (en) | 2012-02-15 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102627955B (en) * | 2012-03-29 | 2013-11-13 | 中国石油天然气集团公司 | High-temperature O2/CO2 corrosion inhibitor for coiled tubing and preparation method of agent B of high-temperature O2/CO2 corrosion inhibitor |
| CN103589413B (en) * | 2012-08-13 | 2016-11-02 | 中国石油天然气股份有限公司 | Oil well acidizing corrosion inhibitor and preparation and application thereof |
| CN103409129B (en) * | 2013-08-09 | 2016-04-27 | 上海富茵环保科技有限公司 | A kind of organic amine drilling well acidification corrosion inhibitor and preparation method thereof |
| CN103898534B (en) * | 2014-03-14 | 2016-03-02 | 杭州央力科技有限公司 | A kind of Mannich base quaternary ammonium salt compound corrosion inhibitor and preparation method thereof |
| CN103966609A (en) * | 2014-05-07 | 2014-08-06 | 广东石油化工学院 | Method for preparing efficient acid-proof corrosion inhibiter |
| CN107573914A (en) * | 2017-08-29 | 2018-01-12 | 中国石油集团渤海钻探工程有限公司 | A kind of compound acidification corrosion inhibitor based on Mannich base and BAA |
| CN107987822A (en) * | 2017-12-06 | 2018-05-04 | 唐山市金沙工贸有限公司 | High-temperature acidification corrosion inhibitor and preparation method thereof and application |
| CN108219905A (en) * | 2017-12-30 | 2018-06-29 | 谢新昇 | A kind of preparation method of permanent seal cooling anticorrosive emulsified oil |
| CN110982508B (en) * | 2019-12-26 | 2022-03-08 | 西南石油大学 | Mannich base acidizing corrosion inhibitor and preparation method thereof |
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