CN112624355A - Multifunctional green group-rich corrosion and scale inhibitor and preparation method thereof - Google Patents

Multifunctional green group-rich corrosion and scale inhibitor and preparation method thereof Download PDF

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Publication number
CN112624355A
CN112624355A CN202011525500.9A CN202011525500A CN112624355A CN 112624355 A CN112624355 A CN 112624355A CN 202011525500 A CN202011525500 A CN 202011525500A CN 112624355 A CN112624355 A CN 112624355A
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China
Prior art keywords
acid
scale inhibitor
corrosion
fulvic acid
solvent
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CN202011525500.9A
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翟洪金
李怀阁
张阳
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Jurong Ningwu New Hi Tech Development Co ltd
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Jurong Ningwu New Hi Tech Development Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
    • C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
    • C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
    • B08B9/027—Cleaning the internal surfaces; Removal of blockages
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B2209/00—Details of machines or methods for cleaning hollow articles
    • B08B2209/02—Details of apparatuses or methods for cleaning pipes or tubes
    • B08B2209/027—Details of apparatuses or methods for cleaning pipes or tubes for cleaning the internal surfaces
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/08—Corrosion inhibition

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)

Abstract

The invention discloses a multifunctional green corrosion and scale inhibitor rich in radicals, which belongs to the field of corrosion and scale inhibitors and mainly comprises two steps of synthesis and compounding: the first is that fulvic acid and organic acid are used as raw materials, and polyacrylic acid fulvic acid ester is synthesized through free radical polymerization and esterification under the action of a catalyst and an initiator. Wherein the fulvic acid accounts for 10-50% of the total mass; the organic acid accounts for 15-55% of the total mass; 0.2 to 3 percent of p-toluenesulfonic acid; 0.1 to 1 percent of initiator; the balance being solvent. Secondly, the polyacrylic acid fulvic acid ester is mixed with a specific synergistic effect substance and a solvent to prepare the green corrosion and scale inhibitor. The mass fraction of each component is as follows: 25-65% of polyacrylic acid fulvic acid ester; the total amount of the synergistic agent is 5-30%; 10-30% of ethanol; the balance of deionized water. The multifunctional and group-rich green corrosion and scale inhibitor has excellent corrosion and scale inhibition performance, has a scale dissolving effect, and meets the requirement of green environmental protection.

Description

Multifunctional green group-rich corrosion and scale inhibitor and preparation method thereof
Technical Field
The invention relates to the field of corrosion and scale inhibitors, in particular to a multifunctional green corrosion and scale inhibitor rich in groups and a preparation method thereof.
Background
The proportion of industrial wastewater and oilfield produced sewage is getting larger and larger nowadays. Calcium salt, magnesium salt, silicate and the like contained in the water lead to scaling and corrosion of pipelines, and the production cost is greatly increased. At present, most of the existing corrosion and scale inhibitors are organic phosphonic acid type scale inhibitors, and the corrosion and scale inhibitors are widely applied by virtue of high-efficiency corrosion and scale inhibition functions, and have the characteristics of stable chemical performance, high temperature and value resistance, obvious solvent limiting effect and synergistic effect and the like. However, phosphorus is a nutrient source of bacteria and algae, and the phosphorus-containing scale inhibitor is easy to cause eutrophication of environmental water areas and promote the growth of bacteria and algae to form red tide to cause water source pollution. Phosphorus prohibition and limitation measures are taken in many countries and regions. The European Union, the United states, Japan, and the like limit the total phosphorus emission concentration to not more than 1.0 mg/L. The discharge standard of pollutants for municipal wastewater treatment plants (GB 18918-2002) in China is also stipulated, and the total phosphorus of the primary discharge standard is less than or equal to 1.0 mg/L. Therefore, the development of a novel green corrosion and scale inhibitor which is phosphorus-free, has good biodegradation performance, simple and easily realized control index and is suitable for high-concentration-ratio operation and even zero pollution discharge has become a development direction of water treatment.
Disclosure of Invention
In order to develop a new corrosion and scale inhibitor single agent and integrally improve the application effect, the invention aims to synthesize polyacrylic acid fulvic acid ester by taking fulvic acid and acrylic acid as raw materials through free radical polymerization and esterification under the action of a catalyst and an initiator, and then mix the polyacrylic acid fulvic acid ester with a synergistic agent, a solvent and the like to prepare the green corrosion and scale inhibitor.
The invention is realized by the following steps:
a preparation method of a multifunctional, rich-group green corrosion and scale inhibitor is characterized in that fulvic acid and organic acid are used as raw materials, polyacrylic acid fulvic acid ester is synthesized through polymerization and esterification of free radicals under the action of a catalyst and an initiator, and then the polyacrylic acid fulvic acid ester is mixed with a synergistic agent and a solvent to prepare the green corrosion and scale inhibitor; the method comprises the following specific steps:
the method comprises the following steps: adding fulvic acid, organic acid, catalyst and initiator into a solvent, stirring and mixing, controlling the temperature to perform polymerization and esterification reaction on free radicals, and judging the reaction end point according to the separated water amount; then, decompressing and distilling off the solvent in the reaction system to obtain the polyacrylic acid fulvic acid ester;
step two: and (3) mixing the polyacrylic acid fulvic acid ester, the synergistic agent, the ethanol and the water in the step one according to a proportion and stirring uniformly.
Further, the mass fractions of the components in the step one are as follows: the fulvic acid accounts for 10-50% of the total mass of the components in the step one; the organic acid accounts for 15-55% of the total mass; the catalyst accounts for 0.2-3% of the total mass; the initiator accounts for 0.1-1% of the total mass; the balance being solvent.
Further, the organic acid is acrylic acid.
Further, the catalyst is p-toluenesulfonic acid; the initiator is azobisisobutyronitrile.
Further, the mass fractions of the components in the second step are as follows: the polyacrylic acid fulvic acid ester accounts for 25-65% of the total mass of the components in the second step; the total amount of the synergistic agent is 5-30%; the total amount of ethanol is 10-30%; the balance of deionized water.
Further, the synergistic agent is polyepoxysuccinic acid.
Further, the polymerization temperature in the method is 30-75 DEGoC, the esterification reaction temperature is 120-150-oAnd C, the esterification reaction solvent is dimethylbenzene, and the using amount of the esterification reaction solvent is 20-60% of the total mass of the reaction materials.
The corrosion and scale inhibitor prepared by the preparation method of the multifunctional green corrosion and scale inhibitor rich in radicals has excellent corrosion and scale inhibition performance, has a scale dissolving effect, and meets the requirement of environmental protection.
Compared with the prior art, the invention has the beneficial effects that:
1. the polyacrylic acid fulvic acid ester synthesized by the invention is a new corrosion and scale inhibitor single agent, the molecular structure contains a large amount of hydroxyl, carbonyl and the like, the linear chain and the branched chain alternately extend, and the molecular weight can be regulated and controlled through the formula design.
2. The corrosion and scale inhibitor is a mixed corrosion and scale inhibitor containing two components, is an environment-friendly corrosion and scale inhibitor, and has a certain scale dissolving effect on scale-formed pipelines.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention more clear, the present invention is further described in detail by the following examples. It should be noted that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention relates to a multifunctional green corrosion and scale inhibitor rich in radicals and a preparation method thereof, which is characterized by comprising the following steps:
the method comprises the following steps: the fulvic acid, the acrylic acid, the catalyst and the initiator are added into a proper solvent to be stirred and mixed, the acrylic acid is polymerized and partially esterified with the fulvic acid under a certain temperature, and the reaction end point is judged according to the separated water amount. Then, decompressing and distilling off the solvent in the reaction system to obtain the polyacrylic acid fulvic acid ester.
Step two: the target product of the patent is obtained by mixing and stirring the polyacrylic acid fulvic acid ester, the synergistic agent, ethanol, water and the like according to a certain proportion.
Specific examples are given below for explanation.
Example 1
Adding 18 g of fulvic acid, 20 g of acrylic acid, 1 g of p-toluenesulfonic acid and 0.5 g of azobisisobutyronitrile into 60 g of dimethylbenzene, stirring and mixing, controlling the mixing speed to be 50 DEGoPolymerizing methacrylic acid at C, 130oC, carrying out partial esterification reaction, and judging the reaction end point according to the separated water amount. Then, decompressing and distilling off the solvent in the reaction system to obtain the polyacrylic acid fulvic acid ester.
Mixing 30 g of polyacrylic acid fulvic acid ester, 25 g of polyepoxysuccinic acid, 20 g of ethanol, 25 g of water and the like, and uniformly stirring to obtain the target product. The specific scale inhibition rate and corrosion inhibition rate of the product are shown in table 1.
Example 2
Adding 24 g of fulvic acid, 30 g of acrylic acid, 1.5 g of p-toluenesulfonic acid and 0.5 g of azobisisobutyronitrile into 44 g of dimethylbenzene, stirring and mixing, and controlling the mixing to be 60 goPolymerizing methacrylic acid at C to obtain 135oC, carrying out partial esterification reaction, and judging the reaction end point according to the separated water amount. Then, decompressing and distilling off the solvent in the reaction system to obtain the polyacrylic acid fulvic acid ester.
Mixing 35 g of polyacrylic acid fulvic acid ester, 20 g of polyepoxysuccinic acid, 15 g of ethanol, 30 g of water and the like, and uniformly stirring to obtain the target product. The specific scale inhibition rate and corrosion inhibition rate of the product are shown in table 1.
Example 3
30 g of fulvic acid, 25 g of acrylic acid, 1 g of p-toluenesulfonic acid and 0.5 g of azobisisobutyronitrile are added into 44 g of xylene and stirred for mixing, and the mixture is controlled to be 60 goPolymerizing methacrylic acid at C to obtain 135oC, carrying out partial esterification reaction, and judging the reaction end point according to the separated water amount. Then, decompressing and distilling off the solvent in the reaction system to obtain the polyacrylic acid fulvic acid ester.
Mixing 40 g of polyacrylic acid fulvic acid ester, 22 g of polyepoxysuccinic acid, 10 g of ethanol, 28 g of water and the like, and uniformly stirring to obtain the target product. The specific scale inhibition rate and corrosion inhibition rate of the product are shown in table 1.
Example 4
10 g of fulvic acid, 55 g of acrylic acid, 0.2 g of p-toluenesulfonic acid and 0.1 g of azobisisobutyronitrile are added into 34.7 g of dimethylbenzene and stirred and mixed, and the mixture is controlled to be 60 goPolymerizing methacrylic acid at C to obtain 135oC, carrying out partial esterification reaction, and judging the reaction end point according to the separated water amount. Then, decompressing and distilling off the solvent in the reaction system to obtain the polyacrylic acid fulvic acid ester.
65 g of polyacrylic acid fulvic acid ester, 20 g of polyepoxysuccinic acid, 10 g of ethanol, 5 g of water and the like are mixed and stirred uniformly to obtain the target product of the patent. The specific scale inhibition rate and corrosion inhibition rate of the product are shown in table 1.
Example 5
50 g of fulvic acid, 15 g of acrylic acid, 3 g of p-toluenesulfonic acid and 1 g of azobisisobutyronitrile are added into 31 g of dimethylbenzene and stirred and mixed, and the mixture is controlled to be 60 goPolymerizing methacrylic acid at C to obtain 135oC, carrying out partial esterification reaction, and judging the reaction end point according to the separated water amount. Then, decompressing and distilling off the solvent in the reaction system to obtain the polyacrylic acid fulvic acid ester.
Mixing 25 g of polyacrylic acid fulvic acid ester, 30 g of polyepoxysuccinic acid, 30 g of ethanol, 15 g of water and the like, and uniformly stirring to obtain the target product. The specific scale inhibition rate and corrosion inhibition rate of the product are shown in table 1.
Example 6
50 g of fulvic acid, 15 g of acrylic acid, 3 g of p-toluenesulfonic acid and 1 g of azobisisobutyronitrile are added into 31 g of dimethylbenzene and stirred and mixed, and the mixture is controlled to be 60 goPolymerizing methacrylic acid at C to obtain 135oC, carrying out partial esterification reaction, and judging the reaction end point according to the separated water amount. Then, decompressing and distilling off the solvent in the reaction system to obtain the polyacrylic acid fulvic acid ester.
65 g of polyacrylic acid fulvic acid ester, 5 g of polyepoxysuccinic acid, 10 g of ethanol, 20 g of water and the like are mixed and stirred uniformly to obtain the target product of the patent. The specific scale inhibition rate and corrosion inhibition rate of the product are shown in table 1.
TABLE 1
Serial number Name (R) The scale inhibition rate% Corrosion inhibition rate%
1 Example 1 product 95 90
2 EXAMPLE 2 product 94 88
3 EXAMPLE 3 product 95 90
4 EXAMPLE 4 product 93 85
5 EXAMPLE 5 product 90 84
6 Example 6 product 92 85
From the above table, it can be seen that the product of the present invention has a high scale inhibition rate and a high corrosion inhibition rate.
The invention provides a multifunctional, group-rich and green corrosion and scale inhibitor and a preparation method thereof, and a plurality of methods and ways for realizing the technical scheme are provided. All the components not specified in the present embodiment can be realized by the prior art.

Claims (8)

1. A preparation method of a multifunctional, rich-group green corrosion and scale inhibitor is characterized in that fulvic acid and organic acid are used as raw materials, polyacrylic acid fulvic acid ester is synthesized through polymerization and esterification of free radicals under the action of a catalyst and an initiator, and then the polyacrylic acid fulvic acid ester is mixed with a synergistic agent and a solvent to prepare the green corrosion and scale inhibitor; the method comprises the following specific steps:
the method comprises the following steps: adding fulvic acid, organic acid, catalyst and initiator into a solvent, stirring and mixing, controlling the temperature to perform polymerization and esterification reaction on free radicals, and judging the reaction end point according to the separated water amount; then, decompressing and distilling off the solvent in the reaction system to obtain the polyacrylic acid fulvic acid ester;
step two: and (3) mixing the polyacrylic acid fulvic acid ester, the synergistic agent, the ethanol and the water in the step one according to a proportion and stirring uniformly.
2. The preparation method of the multifunctional group-rich green corrosion and scale inhibitor according to claim 1, wherein the mass fractions of the components in the first step are as follows: the fulvic acid accounts for 10-50% of the total mass of the components in the step one; the organic acid accounts for 15-55% of the total mass; the catalyst accounts for 0.2-3% of the total mass; the initiator accounts for 0.1-1% of the total mass; the balance being solvent.
3. The method for preparing the multifunctional group-rich green corrosion and scale inhibitor according to claim 2, wherein the organic acid is acrylic acid.
4. The preparation method of the multifunctional group-rich green corrosion and scale inhibitor according to claim 2, wherein the catalyst is p-toluenesulfonic acid; the initiator is azobisisobutyronitrile.
5. The preparation method of the multifunctional group-rich green corrosion and scale inhibitor according to claim 1, wherein the mass fractions of the components in the second step are as follows: the polyacrylic acid fulvic acid ester accounts for 25-65% of the total mass of the components in the second step; the total amount of the synergistic agent is 5-30%; the total amount of ethanol is 10-30%; the balance of deionized water.
6. The preparation method of the multifunctional group-rich green corrosion and scale inhibitor according to claim 5, wherein the synergistic agent is polyepoxysuccinic acid.
7. The method for preparing the multifunctional group-rich green corrosion and scale inhibitor according to claim 1, wherein the polymerization temperature in the method is 30-75%oC, the esterification reaction temperature is 120-150-oAnd C, the esterification reaction solvent is dimethylbenzene, and the using amount of the esterification reaction solvent is 20-60% of the total mass of the reaction materials.
8. A corrosion and scale inhibitor prepared by the preparation method of the multifunctional green corrosion and scale inhibitor rich in radicals according to any one of claims 1 to 7.
CN202011525500.9A 2020-12-22 2020-12-22 Multifunctional green group-rich corrosion and scale inhibitor and preparation method thereof Pending CN112624355A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102464390A (en) * 2011-10-20 2012-05-23 常州亚环环保科技有限公司 Methods for preparation and application of flocculant for treating low-concentration phosphorus-containing wastewater
CN109553200A (en) * 2018-11-21 2019-04-02 句容宁武高新技术发展有限公司 A kind of corrosion inhibiting and descaling agent and preparation method thereof based on modified tannin acid
CN110862495A (en) * 2019-11-12 2020-03-06 句容宁武高新技术发展有限公司 Multifunctional phosphorus-free corrosion and scale inhibitor based on humic acid derivatives and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102464390A (en) * 2011-10-20 2012-05-23 常州亚环环保科技有限公司 Methods for preparation and application of flocculant for treating low-concentration phosphorus-containing wastewater
CN109553200A (en) * 2018-11-21 2019-04-02 句容宁武高新技术发展有限公司 A kind of corrosion inhibiting and descaling agent and preparation method thereof based on modified tannin acid
CN110862495A (en) * 2019-11-12 2020-03-06 句容宁武高新技术发展有限公司 Multifunctional phosphorus-free corrosion and scale inhibitor based on humic acid derivatives and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
聂麦茜: "《有机化学（第2版）》", 31 January 2014, 冶金工业出版社 *

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