CN112176349B - Non-phosphorus corrosion inhibitor composition, non-phosphorus corrosion inhibitor and application thereof - Google Patents
Non-phosphorus corrosion inhibitor composition, non-phosphorus corrosion inhibitor and application thereof Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
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Abstract
The invention relates to the field of corrosion inhibitors, and discloses a phosphorus-free corrosion inhibitor composition, a phosphorus-free corrosion inhibitor and application thereof, wherein the composition comprises a component A, a component B, a component C and a component D, the component A, the component B, the component C and the component D are in a weight ratio of 1: 0.30-8.00: 0.12-3.00: 0.10-2.10, the component A is at least one selected from compounds with a structure shown in a formula (1), the component B is at least one selected from phosphorus-free corrosion inhibition polymers, the component C is at least one selected from organic acids and organic acid salts, and the component D is at least one selected from water-soluble zinc salts. The corrosion inhibitor composition has good corrosion inhibition effect, can achieve better corrosion inhibition effect under the condition of lower corrosion inhibitor concentration without influencing treatment effect, and greatly saves cost.
Description
Technical Field
The invention relates to the field of corrosion inhibitors, in particular to a phosphorus-free corrosion inhibitor composition, a phosphorus-free corrosion inhibitor and application of the phosphorus-free corrosion inhibitor in inhibiting corrosion of carbon steel in seawater.
Background
Petrochemical enterprises are industrial water consumers, and with the rapid development of industry and agriculture, the demand of fresh water resources is increasing, so that the fresh water resources are increasingly deficient. Of the industrial water usage, about 70% is used for industrial cooling. The seawater has the advantages of low water taking temperature, small influence of seasons, good cooling effect, sufficient water source and the like, so if the seawater can be used for replacing fresh water for industrial circulating cooling water, the seawater cooling device has important significance for relieving the situation of shortage of fresh water resources in China.
The seawater has complex components and high salt content, particularly has extremely high chloride ion content, so the seawater is much more corrosive than fresh water. The main problems of using seawater as circulating water cooling water are serious corrosion, easy scaling and biological attachment. The strong corrosivity of seawater is the main reason for causing the corrosion of circulating water system pipelines and heat exchange equipment, so the key point for solving the corrosion of carbon steel in seawater is that seawater is used for circulating cooling water. The addition of corrosion inhibitors is an effective method for solving the problem.
The corrosion and scale inhibitor formula used in cooling water treatment in China is mainly a phosphorus-based formula, and although the performance of the corrosion and scale inhibitor formula can basically meet the use requirements, the phosphorus-based formula still has the following defects: the phosphorus water treatment agent has the hidden trouble of easily forming phosphate scale in the using process, and influences the heat exchange effect of the water cooler during long-term operation; the phosphorus formula promotes the propagation of microorganisms in the circulating water, and a large amount of bactericide is consumed; the discharge of a large amount of phosphorus easily causes eutrophication of the receiving water body. Therefore, the development and use of a low-phosphorus or phosphorus-free corrosion and scale inhibitor formula have important significance for cooling water treatment.
CN107829091A discloses an environment-friendly carbon steel corrosion inhibitor containing crop straw solid extract, which comprises the following raw materials in percentage by weight: 40-60 parts of crop straw solid extract, 1-5 parts of hydroxyethyl methacrylate, 5-10 parts of zinc sulfate, 1-5 parts of sodium silicate and 1-2 parts of sodium molybdate, although the carbon steel corrosion inhibition rate is high, the extraction process of the crop straw solid extract is complicated, and a large amount of organic solvent is required in the extraction process.
CN101618914A discloses a tungstate composite seawater corrosion inhibitor suitable for seawater as circulating cooling water, which is characterized in that: based on 1L of seawater, according to the mass concentration ratio, 40mg/L of tungstate, 40mg/L of polyepoxysuccinic acid, 10mg/L of sodium gluconate and 4mg/L of zinc salt are respectively taken. In the prior art, although the corrosion inhibition rate of the composite corrosion inhibitor is higher, the consumption of the corrosion inhibitor is larger, and the cost of tungstate is higher, so that the cost of the corrosion inhibitor is higher.
Disclosure of Invention
The invention aims to save cost by effectively reducing the consumption of the corrosion inhibitor on the premise of not influencing the corrosion inhibition effect.
In order to achieve the above object, a first aspect of the present invention provides a phosphorus-free corrosion inhibitor composition, which contains component a, component B, component C, and component D at a weight ratio of 1: 0.30-8.00: 0.12-3.00: 0.10, wherein component a is at least one selected from compounds having a structure represented by formula (1), component B is at least one selected from phosphorus-free corrosion inhibiting polymers, component C is at least one selected from organic acids and organic acid salts, and component D is at least one selected from water-soluble zinc salts,
wherein, in the formula (1), R1is-H, -COOH or phenyl; r2is-H, -CH2COOH or C1-C5A lower alkyl group of (a);
the polymerization degree x is 1-5000; the polymerization degree y is 1-5000; the polymerization degree n is 1-100.
In a second aspect, the present invention provides a phosphorus-free corrosion inhibitor, which comprises a phosphorus-free corrosion inhibitor composition and water, wherein the phosphorus-free corrosion inhibitor composition is the composition described in the first aspect of the present invention.
A third aspect of the invention provides the use of a corrosion inhibitor as described in the second aspect above for inhibiting corrosion of carbon steel in seawater.
The compound with the structure shown in the formula (1) provided by the invention has good corrosion inhibition effect, and can achieve better corrosion inhibition effect under the condition of lower corrosion inhibitor concentration on the premise of not influencing treatment effect, thereby greatly saving cost.
Moreover, the inventor of the invention finds that the components A, B, C and D in the formula have synergistic effect, so that the use amount of each single agent is reduced, and the operation cost can be obviously reduced.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and these ranges or values should be understood to encompass values close to these ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the present invention, "at least one" means one or a mixture of two or more.
As described above, in a first aspect, the present invention provides a phosphorus-free corrosion inhibitor composition, which contains component a, component B, component C, and component D at a weight ratio of 1: (0.30-8.00): 0.12-3.00): 0.10-2.10, wherein component a is selected from at least one of compounds having a structure represented by formula (1), component B is selected from at least one of phosphorus-free corrosion-inhibiting polymers, component C is selected from at least one of organic acids and organic acid salts, and component D is selected from at least one of water-soluble zinc salts,
wherein, in the formula (1), R1is-H, -COOH or phenyl; r2is-H, -CH2COOH or C1-C5A lower alkyl group of (a);
the polymerization degree x is 1-5000; the polymerization degree y is 1-5000; the polymerization degree n is 1-100.
In a preferred embodiment of the invention, R1is-H, R2is-H; or R1is-COOH, R2is-H; or R1is-H, R2is-CH2COOH; or R1is-H, R2Is C1-C5The lower alkyl group of (2). Preferably, R is selected to further enhance the corrosion inhibiting effect of the phosphorus-free corrosion inhibitor composition1is-COOH, R2is-H.
Wherein, in the formula (1), the polymerization degree x is 1 to 5000, preferably 10 to 200; the degree of polymerization y is 1 to 5000, preferably 10 to 200; the degree of polymerization n is from 1 to 100, preferably from 5 to 55.
Particularly preferably, the weight average molecular weight of the compound having the structure represented by the formula (1) is 1000-300000, more preferably 10000-270000.
Preferably, the weight ratio of the components A, B, C and D is 1: 0.75-5.00: 0.20-2.00: 0.15-1.60, in order to further improve the corrosion inhibition effect.
Preferably, the phosphorus-free corrosion-inhibiting polymer is polyaspartic acid, polyepoxysuccinic acid, and hydrolyzed polymaleic anhydride.
Preferably, the organic acid is an ascorbic acid compound. Particularly preferably, the ascorbyl compound is selected from at least one of ascorbic acid, dehydroascorbic acid, erythorbic acid and dehydroerythorbic acid.
Preferably, the organic acid salt is a gluconate compound. Particularly preferably, the gluconate-type compound is selected from at least one of sodium gluconate, potassium gluconate, sodium D-gluconate, potassium D-gluconate, zinc gluconate and manganese gluconate.
According to a particularly preferred embodiment, component C is selected from at least one of organic acid salts.
In the invention, the water-soluble zinc salt can be various water-soluble inorganic zinc salts which are conventionally used in the field of water treatment agents. Preferably, the water-soluble zinc salts are zinc chloride, zinc sulfate and zinc nitrate; in order to further increase the corrosion inhibition effect, zinc sulfate and/or zinc chloride are particularly preferred.
According to a preferred embodiment, the compound of formula (1) is prepared by a process comprising the steps of:
(1) under the esterification condition, contacting allyloxy polyethylene glycol with maleic anhydride for reaction to obtain allyloxy polyethylene glycol maleic acid monoester;
(2) contacting the allyloxy polyethylene glycol maleic acid monoester obtained in the step (1) with unsaturated carboxylic acid and an initiator to react under the condition of free radical copolymerization and in the presence of water.
In the esterification reaction stage, the weight average molecular weight of the allyloxy polyethylene glycol is preferably 230-2500, namely 4-55 polyethylene glycol repeating units, and the weight average molecular weight is preferably 320-1100, namely 6-24 polyethylene glycol repeating units.
According to the present invention, in step (1), the esterification reaction conditions generally include a reaction temperature and a reaction time, the reaction temperature may be 70 to 120 ℃, more preferably 80 to 100 ℃, and the reaction time may be 1 to 6 hours. The molar ratio of maleic anhydride to allyloxypolyoxyethylene ether is preferably 1: 0.9-1.1.
According to the present invention, it is preferable that the method of contacting the allyloxypolyethylene glycol maleic acid monoester and the unsaturated carboxylic acid with the initiator in the presence of water in the step (2) comprises: mixing allyloxy polyethylene glycol maleic acid monoester with unsaturated carboxylic acid and water, heating to 55-80 ℃, and then dropwise adding an initiator.
According to the present invention, in the step (2), the radical copolymerization conditions generally include a reaction temperature and a reaction time, the reaction temperature may be 75 to 110 ℃, and the reaction time may be 1 to 10 hours.
According to the present invention, in the step (2), the mass ratio of the allyloxypolyethylene glycol maleic acid monoester to the unsaturated carboxylic acid may be 95:5 to 5:95, and water is used as the solvent as long as sufficient dissolution of the reactant is ensured, and preferably, the mass of water is 0.5 to 10 times the total mass of the allyloxypolyethylene glycol maleic acid monoester and the unsaturated carboxylic acid.
According to the present invention, the unsaturated carboxylic acid is selected from a wide range, and in order to further improve the corrosion inhibition effect of the composition of the present invention, the unsaturated carboxylic acid is selected from one or more of acrylic acid, methacrylic acid, maleic anhydride, itaconic acid and cinnamic acid, and more preferably, the unsaturated carboxylic acid is maleic acid and/or maleic anhydride.
According to the present invention, the initiator is preferably selected from one or more of ammonium persulfate, sodium persulfate, and potassium persulfate. The initiator is generally used in the form of an aqueous initiator solution, the concentration and amount of which are conventional in the art. For example, the mass fraction of the aqueous initiator solution may be 5 to 50%, and preferably, the mass of the initiator in the aqueous initiator solution is 0.01 to 0.2 times the total mass of the allyloxypolyethylene glycol maleic acid monoester and the unsaturated carboxylic acid, and the dropping time of the initiator is preferably 0.25 to 5 hours.
As mentioned above, in a second aspect of the present invention, there is provided a phosphorus-free corrosion inhibitor comprising a phosphorus-free corrosion inhibitor composition and water, the phosphorus-free corrosion inhibitor composition being the composition of the first aspect of the present invention.
Preferably, the non-phosphorus corrosion inhibitor composition is present in an amount of 20 to 90 wt.%, more preferably 45 to 80 wt.%, based on the total weight of the corrosion inhibitor.
According to a preferred embodiment, in the phosphorus-free corrosion inhibitor of the present invention, the content of component a is 5 to 50 wt.% based on the total amount of the phosphorus-free corrosion inhibitor; the content of the component B is 10-40 wt%; the content of the component C is 2.5-20 wt%; the content of the component D is 4-9 wt%, and the balance is water.
As mentioned above, a third aspect of the invention provides the use of a corrosion inhibitor according to the second aspect as defined above for inhibiting corrosion of carbon steel in seawater.
Preferably, the amount of corrosion inhibitor is 75-145mg, preferably 90-110mg, per litre of seawater.
The present invention will be described in detail below by way of examples. In the following examples, various raw materials used are commercially available ones unless otherwise specified.
The test water used in the examples was sea water in Bohai Bay, and the water quality is shown in Table 1.
Table 1: main water quality of Bohai Bay seawater
The method for detecting the corrosion inhibition performance of the corrosion inhibitor in the following examples refers to methods 401, 402, 403 and 404 in the analysis and test method of cooling water (1993, published by the information center of the Chongqing petrochemical industry general factory) written by the Ministry of production and development of the general chemical industries of China. Wherein, the dosage of the corrosion inhibitor is 100mg relative to each liter of Bohai Bay seawater.
In the following examples, the average corrosion rate is defined as the corrosion inhibition efficiency of the corrosion inhibitor, and the average corrosion rate is calculated by the formula:
Preparation example 1
Allyloxypolyethylene glycol (0.01mol) with molecular weight of 278 (namely n-5) and maleic anhydride (0.01mol) are added into a reaction kettle for esterification reaction at the temperature of 70 ℃ for 2h to generate allyloxypolyethylene glycol maleic acid monoester.
Adding 1g of acrylic acid and 20g of distilled water into a reaction kettle, uniformly stirring, dropwise adding 1g of 10 mass percent ammonium persulfate aqueous solution at 60 ℃ for 15min, heating to 80 ℃ after dropwise adding, reacting for 1h, and cooling to room temperature to obtain a yellow solution, namely a compound A1 with the structure shown in the formula (1) and the weight-average molecular weight of 1.89 multiplied by 105。
Preparation example 2
Allyloxypolyethylene glycol (0.01mol) with the molecular weight of 498 (namely n-10) and maleic anhydride (0.01mol) are added into a reaction kettle for esterification reaction at the temperature of 80 ℃ for 3h to generate allyloxypolyethylene glycol maleic acid monoester.
Adding 2g of acrylic acid and 20g of distilled water into a reaction kettle, uniformly stirring, dropwise adding 2g of 10 mass percent ammonium persulfate aqueous solution at 60 ℃ for 30min, heating to 80 ℃ after dropwise adding, reacting for 2h, and cooling to room temperature to obtain a yellow solution, namely the compound A2 with the structure shown in the formula (1) and the weight-average molecular weight of 1.48 multiplied by 105。
Preparation example 3
Allyloxypolyethylene glycol (0.01mol) with the molecular weight of 498 (namely n-10) and maleic anhydride (0.01mol) are added into a reaction kettle for esterification reaction at the temperature of 80 ℃ for 3h to generate allyloxypolyethylene glycol maleic acid monoester.
Adding 2g of maleic anhydride and 20g of distilled water into a reaction kettle, uniformly stirring, dropwise adding 2g of 10 mass percent ammonium persulfate aqueous solution at 65 ℃, dropwise adding for 30min, heating to 80 ℃ after dropwise adding, reacting for 3h, cooling to room temperature to obtain a yellow solution, namely a compound A3 with the structure shown in the formula (1), wherein the weight average molecular weight is 2.58 multiplied by 105。
Examples
Weighing the component D, placing the component D in a beaker, adding water, stirring and dissolving, then adding the component A, the component B and the component C, and stirring uniformly to obtain the corrosion inhibitor.
The species and amounts of substances in the examples are shown in table 2.
Comparative example 1
Weighing 40g of sodium tungstate, 40g of polyepoxysuccinic acid, 10g of sodium gluconate, 4g of zinc chloride and 6g of water, and uniformly stirring to obtain the corrosion inhibitor DH 1.
Comparative example 2
Weighing 8.6g of zinc sulfate, placing the zinc sulfate in a 250mL beaker, adding 41.9g of deionized water, stirring to dissolve, then adding 37.5g of polyepoxysuccinic acid and 12g of sodium gluconate, and stirring uniformly to obtain the corrosion inhibitor DH 2.
Comparative example 3
The formulations were prepared in the same manner as in the examples, except that the amount or kind of the substance was varied as shown in Table 2.
Comparative example 4
Prepared in the same manner as in the examples, except that the amount or kind of the substance used was varied, as shown in Table 2, wherein DA1 was a commercially available acrylic acid-2-acrylamido-2-methylpropanesulfonic acid polymer (AA-AMPS, available from Shandong Tai and Co.).
Comparative example 5
Prepared by the same method as in the example, except that the amount or kind of the substance is different, specifically as shown in table 2, wherein DA2 is acrylic acid-allyloxy polyoxyethylene sulfonate copolymer AA-APES prepared according to the published literature (synthesis and performance studies of AA/APES scale inhibitors, wuyuanhong, etc., chemist-hour publication, 2010, 24(5), 12-14).
The compositions of each example and some of the comparative examples are shown in table 2.
TABLE 2
Test example
The corrosion inhibitors obtained in the examples and comparative examples were evaluated for corrosion inhibition performance, respectively, and the results are shown in Table 3.
TABLE 3
| Item | Corrosion Rate (mm/a) |
| Example 1 | 0.0120 |
| Example 2 | 0.0122 |
| Example 3 | 0.0125 |
| Example 4 | 0.0133 |
| Example 5 | 0.0137 |
| Example 6 | 0.0120 |
| Comparative example 1 | 0.0138 |
| Comparative example 2 | 0.0350 |
| Comparative example 3 | 0.0300 |
| Comparative example 4 | 0.0220 |
| Comparative example 5 | 0.0272 |
From the results in table 3, it can be seen that the corrosion rate of the corrosion inhibitor of the present invention is significantly reduced, while the corrosion rate of the prior art without the use of the corrosion inhibitor of the present invention is significantly increased.
In addition, although the corrosion inhibitor in the comparative example 1 can obtain the corrosion inhibition performance obviously superior to that of the comparative example 2, a large amount of sodium tungstate with obviously higher cost is required to be applied, and the industrial production application is not facilitated.
Therefore, the phosphorus-free corrosion inhibitor composition effectively reduces the consumption of the corrosion inhibitor and saves the cost.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (19)
1. A non-phosphorus corrosion inhibitor composition comprises a component A, a component B, a component C and a component D, wherein the component A, the component B, the component C and the component D are in a weight ratio of 1: 0.30-8.00: 0.12-3.00: 0.10, the component A is at least one of compounds with a structure shown in a formula (1), the component B is at least one of non-phosphorus corrosion inhibition polymers, the component C is at least one of organic acid and organic acid salt, the organic acid component D is at least one of water-soluble zinc salt,
wherein, in the formula (1), R1is-H, -COOH or phenyl; r2is-H, -CH2COOH or C1-C5A lower alkyl group of (a);
the polymerization degree x is 1-5000; the polymerization degree y is 1-5000; the polymerization degree n is 1-100.
2. The composition according to claim 1, wherein, in formula (1), R1is-COOH, R2is-H.
3. The composition according to claim 1, wherein, in formula (1), the degree of polymerization x is 10 to 200; the polymerization degree y is 10-200; the polymerization degree n is 5-55.
4. The composition as claimed in claim 1, wherein the compound having the structure represented by formula (1) has a weight average molecular weight of 1000-300000.
5. The composition according to any one of claims 1 to 4, wherein the weight ratio of component A, component B, component C and component D is 1: (0.75-5.00): (0.20-2.00): 0.15-1.60).
6. The composition of any one of claims 1-4, wherein the phosphorus-free corrosion-inhibiting polymer is polyaspartic acid, polyepoxysuccinic acid, and hydrolyzed polymaleic anhydride.
7. The composition of any one of claims 1-4, wherein the organic acid is an ascorbate compound; the organic acid salt is a gluconate compound.
8. The composition of claim 7, wherein the organic acid is selected from at least one of ascorbic acid, dehydroascorbic acid, erythorbic acid, and dehydroerythorbic acid; the organic acid salt is at least one selected from sodium gluconate, potassium gluconate, D-sodium gluconate, D-potassium gluconate, zinc gluconate and manganese gluconate.
9. The composition according to any one of claims 1 to 4, wherein the component C is at least one selected from organic acid salts.
10. The composition of any of claims 1-4, wherein the water soluble zinc salt is zinc chloride, zinc sulfate, and zinc nitrate.
11. The composition according to any one of claims 1 to 4, wherein the compound having the structure represented by formula (1) is prepared by a method comprising the steps of:
(1) under the esterification condition, contacting allyloxy polyethylene glycol with maleic anhydride for reaction to obtain allyloxy polyethylene glycol maleic acid monoester;
(2) contacting the allyloxy polyethylene glycol maleic acid monoester obtained in the step (1) with unsaturated carboxylic acid and an initiator to react under the condition of free radical copolymerization and in the presence of water.
12. The composition of claim 11, wherein in step (1), the esterification conditions comprise: the reaction temperature is 70-120 ℃, and the reaction time is 1-6 h; the molar ratio of the maleic anhydride to the allyloxy polyethylene glycol is 1: 0.9-1.1.
13. The composition of claim 11, wherein in step (2), the method of contacting the allyloxypolyethylene glycol maleic acid monoester with the unsaturated carboxylic acid and the initiator in the presence of water comprises: mixing allyloxy polyethylene glycol maleic acid monoester with unsaturated carboxylic acid and water, heating to 55-80 ℃, and then dropwise adding an initiator.
14. A phosphorus-free corrosion inhibitor comprising a phosphorus-free corrosion inhibitor composition and water, the phosphorus-free corrosion inhibitor composition being the composition of any one of claims 1-13.
15. The corrosion inhibitor according to claim 14, wherein the phosphorus-free corrosion inhibitor composition is present in an amount of 20 to 90 wt.%, based on the total weight of the corrosion inhibitor.
16. The corrosion inhibitor of claim 15, wherein the phosphorus-free corrosion inhibitor composition is present in an amount of 45 to 80 wt.%, based on the total weight of the corrosion inhibitor.
17. Use of a corrosion inhibitor as claimed in any one of claims 14 to 16 for inhibiting corrosion of carbon steel in seawater.
18. Use according to claim 17, wherein the corrosion inhibitor is used in an amount of 75-145mg per litre of seawater.
19. Use according to claim 18, wherein the corrosion inhibitor is used in an amount of 90-110mg per litre of seawater.
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