CN111809186A - Closing agent and preparation method and application thereof - Google Patents
Closing agent and preparation method and application thereof Download PDFInfo
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- CN111809186A CN111809186A CN202010482646.3A CN202010482646A CN111809186A CN 111809186 A CN111809186 A CN 111809186A CN 202010482646 A CN202010482646 A CN 202010482646A CN 111809186 A CN111809186 A CN 111809186A
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- parts
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- amine compound
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- C—CHEMISTRY; METALLURGY
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- 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
- C23F11/14—Nitrogen-containing compounds
- C23F11/141—Amines; Quaternary ammonium compounds
- C23F11/143—Salts of amines
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention provides a closing agent and a preparation method and application thereof, wherein the closing agent comprises the following raw materials in parts by weight: 30-45 parts of organic dibasic acid, 18-31 parts of alcohol amine compound, 5-15 parts of ammonium citrate and 20-30 parts of deionized water. Under the action of ammonium citrate, organic dibasic acid and an alcohol amine compound react to generate a mixture of ester and amide, the mixture is interwoven into a reticular film, and the film is complexed with metal ions and adsorbed on the surface of metal; meanwhile, the ammonium citrate also has the function of a pH buffering agent, promotes the complexation of the film and metal ions and plays a role in protecting the film. The raw materials can play a synergistic effect: on one hand, the toughness of the film is improved, on the other hand, the complexing degree of the film and metal ions can be improved, so that the film is effectively prevented from being dissolved or washed away under the impact of water or high-temperature condition, the scaling is effectively prevented, the stable water quality is kept, and the water treatment method can be applied to a circulating water system.
Description
Technical Field
The invention relates to the technical field of water circulation systems, in particular to a closing agent and a preparation method and application thereof.
Background
When the metal is in contact with the surrounding medium, chemical or electrochemical action often occurs, for example, when the water circulation system is in operation, a mixture of water and steam continuously and regularly circulates in a closed loop, and heat absorbed by a heated surface in the water circulation system is continuously taken away by the flowing mixture of water and steam to ensure the temperature of the circulating water. However, since the water contains ions such as calcium, magnesium, iron, aluminum, and zinc, solid deposits are firmly attached to the heated surface or the part where the flow of water is slow in the water circulation system, and cannot be discharged in time, and thus, the solid deposits are converted into scale. The heat conductivity coefficient of the scale is poor, so that the heat transfer effect is seriously hindered, and fuel is wasted; corrode the equipment of the water circulation and shorten its life; and even blocking the pipes of the water circulation system, causing accidents. Therefore, prevention of corrosion scaling is a necessary condition for ensuring safe operation of the water circulation system.
Most of the existing methods for preventing corrosion and scale formation on metal surfaces adopt rust inhibitors or corrosion inhibitors, for example, chinese patent document CN105463472A discloses a water-soluble rust inhibitor, which specifically comprises fatty acid, specific amine, additive, ethanol and water, wherein the weight ratio of the fatty acid, the alcohol amine, the additive, the ethanol and the water is: 2-3: 1-15: 5-10: 10-15: 80-100, wherein the fatty acid is selected from one or more of oxalic acid, valeric acid, naphthenic acid, citric acid, benzoic acid, lauric acid, adipic acid, oleic acid and sebacic acid, the specific amine is selected from one or more of caprylic acid dicyclohexylamine, triethanolamine, diethanolamine and ethanolamine, and the additive is an antioxidant.
The water-soluble rust inhibitor disclosed in the above documents can be attached to a metal surface, and forms a rust-proof film of only several tens of micrometers on the metal surface, has good abrasion resistance and rust-proof performance, and is low in production cost, free from extraneous odor, and favorable for environmental protection. However, the rust inhibitor can only be applied to metal surfaces, and has no rust inhibiting property in the face of liquid water or other severe environmental factors, such as in a water circulation system.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect that the antirust agent in the prior art is not suitable for a water circulation system, thereby providing a closing agent, a preparation method and application thereof.
Therefore, the invention provides the following technical scheme:
the closure agent comprises the following raw materials in parts by weight: 30-45 parts of organic dibasic acid, 18-31 parts of alcohol amine compound, 5-15 parts of ammonium citrate and 20-30 parts of deionized water.
Further, the organic dibasic acid is sebacic acid and/or adipic acid;
the alcohol amine compound is triethanolamine and/or ethanolamine.
Further, the closure agent comprises the following raw materials in parts by weight:
20-25 parts of sebacic acid, 10-20 parts of adipic acid, 15-25 parts of triethanolamine, 3-6 parts of ethanolamine, 5-15 parts of ammonium citrate and 20-30 parts of deionized water.
The invention also provides a preparation method of the occlusive agent, which comprises the following steps:
and (3) uniformly mixing deionized water and ammonium citrate, sequentially adding organic dibasic acid and an alcohol amine compound, and stirring to obtain the closer.
Further, the addition temperature of the organic dibasic acid is 75-85 ℃.
Further, after adding the organic dibasic acid, heating to 85-90 ℃, stirring for 25-35 min, and then adding the alcohol amine compound.
Further, the adding temperature of the alcohol amine compound is 90-97 ℃.
Further, after the addition of the alcohol amine compound is finished, stirring is continued for 55-65 min, the temperature is reduced to 85-90 ℃, stirring is continued for 350-370 min, and then the temperature is naturally reduced to the room temperature.
Further, when more than one alcohol amine compound is added, the alcohol amine compound is added separately, and the adding time interval is 110-130 min.
The invention also provides the application of the occlusive agent or the occlusive agent prepared by the preparation method of the occlusive agent in a water circulation system.
The technical scheme of the invention has the following advantages:
1. the inventor researches that the existing antirust agent or corrosion inhibitor for preventing the scaling of the metal surface is mostly not suitable for a water circulation system, and the effective period is only 1-2 years generally, and the inventor believes that the main reason is that the existing antirust agent or corrosion inhibitor is mostly combined with the metal surface through covalent bonds and/or coordination bonds to form a film, so that the metal in water is corroded, and the combination force between the metal and the film is poor, so that when the antirust agent or corrosion inhibitor is applied to the water circulation system, the film combined on the metal surface is easily washed away under the impact of flowing water; even at high temperatures, the thin film bonded to the metal surface dissolves in water.
The invention provides a closure agent, which comprises the following raw materials in parts by weight: 30-45 parts of organic dibasic acid, 18-31 parts of alcohol amine compound, 5-15 parts of ammonium citrate and 20-30 parts of deionized water. Under the action of ammonium citrate, organic dibasic acid and an alcamines compound react to generate a mixture of ester and amide and are interwoven into a film, the film can chelate calcium and magnesium ions in water to prevent the calcium and magnesium ions from being separated out, and the film can be adsorbed on the surface of metal to protect the metal; meanwhile, the ammonium citrate in the raw materials also has the function of a pH buffering agent, promotes the adsorption of the film and the metal surface and plays a role in protecting the film. The closure agent provided by the invention can play a synergistic effect by adopting the raw materials and limiting the mixture ratio of the raw materials: not only can not corrode metal in water, but also can protect the metal: on one hand, the formed scale has a certain decomposition effect, the water quality in a fully-sealed circulating system can be kept from scaling within 3-4 years (the period is not increased continuously), on the other hand, the toughness of the film and the adsorption force between the film and the metal surface can be improved, so that the film is effectively prevented from being dissolved or washed off under the impact of water or high-temperature conditions, the scale is effectively prevented, the circulating water has the characteristics of high temperature resistance and oxidation resistance, the water quality is kept stable, the circulating water can be applied to a circulating water system, and the circulating water added with the closing agent still meets the comprehensive wastewater discharge standard of GB 8978-1996 after the closing agent fails.
2. The invention provides a closing agent, which is prepared by limiting the organic dibasic acid to be sebacic acid and/or adipic acid; the alcohol amine compound is triethanolamine and/or ethanolamine; the toughness of the film and the complexing degree of the film and metal ions in water can be further improved, and the high temperature resistance and oxidation resistance of the film are improved.
3. The closing agent provided by the invention has the advantages that the anti-scaling effect of the closing agent in a circulating water system can be obviously improved and the water quality is kept stable by limiting 20-25 parts of sebacic acid, 10-20 parts of adipic acid, 15-25 parts of triethanolamine, 3-6 parts of ethanolamine, 5-15 parts of ammonium citrate and 20-30 parts of deionized water.
4. The preparation method of the occlusive agent provided by the invention comprises the following steps: and (3) uniformly mixing deionized water and ammonium citrate, sequentially adding organic dibasic acid and an alcohol amine compound, and stirring to obtain the closer. Under the catalysis of ammonium citrate, organic dibasic acid and alcohol amine compounds react to generate a mixture of ester and amide, and the mixture is interwoven into a reticular film, and the film is adsorbed on the surface of metal through the complexation with metal ions; meanwhile, the ammonium citrate also has the function of a pH buffering agent, promotes the complexation of the film and metal ions, plays a role in protecting the film, and prevents the film from being damaged due to too strong acidity. By limiting the feeding sequence of the raw materials, the prepared closer not only can not corrode metal in water, but also can protect the metal: on one hand, the scale remover has certain decomposition effect on formed scale, so that the water quality can not be scaled within 6-7 years; on the other hand, the toughness of the film and the complexing degree of the film and metal ions can be improved, so that the film is effectively prevented from being dissolved or washed away under the impact of water or high-temperature conditions, the scaling is effectively prevented, the water quality is kept stable, and the water circulating system can be applied to a circulating water system.
5. The preparation method of the closing agent provided by the invention can further improve the toughness of a film formed in the later period and prevent pitting corrosion on the film by limiting the adding sequence of the organic dibasic acid.
6. The preparation method of the closing agent provided by the invention can further improve the toughness of the film and the characteristics of high temperature resistance and oxidation resistance of the closing agent by limiting the stirring temperature and time after the organic dibasic acid is added and the adding temperature of the alcohol amine compound.
7. According to the preparation method of the closer provided by the invention, the performances of preventing scaling, resisting high temperature and keeping stable water quality of the prepared closer in a circulating water system can be further improved by limiting the adding time interval of the alcohol amine compound and the stirring time after the alcohol amine compound is added.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
This example provides a closure agent prepared as follows:
uniformly mixing 25kg of deionized water and 10kg of ammonium citrate, adding 20kg of sebacic acid and 20kg of adipic acid at 80 ℃, heating to 90 ℃, and stirring for 30 min; and continuously adding 15kg of triethanolamine, heating to 97 ℃, stirring for 120min, adding 5kg of ethanolamine, continuously stirring for 60min, cooling to 90 ℃, stirring for 360min, and naturally cooling to room temperature to obtain the closer.
Example 2
This example provides a closure agent prepared as follows:
uniformly mixing 20kg of deionized water and 15kg of ammonium citrate, adding 25kg of sebacic acid and 15kg of adipic acid at 75 ℃, heating to 85 ℃, and stirring for 25 min; and continuously adding 20kg of triethanolamine, heating to 90 ℃, stirring for 110min, then adding 3kg of ethanolamine, continuously stirring for 65min, then cooling to 85 ℃, stirring for 350min, and naturally cooling to room temperature to obtain the closer.
Example 3
This example provides a closure agent prepared as follows:
uniformly mixing 30kg of deionized water and 5kg of ammonium citrate, adding 23kg of sebacic acid and 10kg of adipic acid at 85 ℃, heating to 88 ℃, and stirring for 35 min; and continuously adding 25kg of triethanolamine, heating to 95 ℃, stirring for 130min, adding 6kg of ethanolamine, continuously stirring for 55min, cooling to 88 ℃, stirring for 370min, and naturally cooling to room temperature to obtain the closer.
Example 4
This example provides a closure agent prepared as follows:
uniformly mixing 25kg of deionized water and 10kg of ammonium citrate, adding 20kg of sebacic acid at 80 ℃, heating to 90 ℃, and stirring for 30 min; and continuously adding 15kg of triethanolamine, heating to 97 ℃, stirring for 120min, adding 5kg of ethanolamine, continuously stirring for 60min, cooling to 90 ℃, stirring for 360min, and naturally cooling to room temperature to obtain the closer.
Example 5
This example provides a closure agent prepared as follows:
uniformly mixing 25kg of deionized water and 10kg of ammonium citrate, adding 20kg of sebacic acid and 20kg of adipic acid at 80 ℃, heating to 90 ℃, and stirring for 30 min; and continuously adding 15kg of triethanolamine, heating to 97 ℃, stirring for 120min, cooling to 90 ℃, stirring for 360min, and naturally cooling to room temperature to obtain the closer.
Example 6
This example provides a closure agent prepared as follows:
uniformly mixing 25kg of deionized water and 10kg of ammonium citrate, adding 20kg of adipic acid at 80 ℃, heating to 90 ℃, and stirring for 30 min; adding 5kg of ethanolamine, heating to 97 ℃, continuously stirring for 60min, cooling to 90 ℃, stirring for 360min, and naturally cooling to room temperature to obtain the closer.
Comparative example 1
The present comparative example provides a occlusive agent, which is prepared by the following method:
uniformly mixing 25kg of deionized water, 20kg of sebacic acid and 20kg of adipic acid at 80 ℃, and then heating to 90 ℃ and stirring for 30 min; and continuously adding 15kg of triethanolamine, heating to 97 ℃, stirring for 120min, adding 5kg of ethanolamine, continuously stirring for 60min, cooling to 90 ℃, stirring for 360min, and naturally cooling to room temperature to obtain the closer.
Comparative example 2
The present comparative example provides a occlusive agent, which is prepared by the following method:
uniformly mixing 25kg of deionized water and 10kg of citric acid, adding 20kg of sebacic acid and 20kg of adipic acid at 80 ℃, heating to 90 ℃, and stirring for 30 min; and continuously adding 15kg of triethanolamine, heating to 97 ℃, stirring for 120min, adding 5kg of ethanolamine, continuously stirring for 60min, cooling to 90 ℃, stirring for 360min, and naturally cooling to room temperature to obtain the closer.
Experimental example 1
The closure agent prepared in each example and comparative example is mixed with underground water according to the mass ratio of 1: 30, uniformly mixing to obtain a mixed solution; and then respectively putting 500g of the mixed solution and 500g of underground water into 1000ml of beakers with the same specification, heating and evaporating at 100 ℃, cooling to room temperature after boiling for 30min, weighing the mass of the volatilized water if the mixed solution is transparent and uniform through visual observation, supplementing the underground water in an equal amount, continuing heating and evaporating, and circulating the steps until floccules are generated after cooling. The specific experimental results are shown in table 1.
TABLE 1 results of the experiment
The data in the table show that the closer provided by the invention has strong complexing ability against hard water in a water circulation system, and can promote the chelation of calcium, magnesium and other ions in water and metals, so that the water quality is not scaled and the water quality is kept stable.
Experimental example 2
The closing agent prepared in each example and each comparative example is mixed with corrosive water according to the mass ratio of 1: 30, uniformly mixing to obtain a mixed solution; the mixed solution is tested by respectively referring to a GB/T18175-2014 water treatment agent corrosion inhibition performance determination-rotary hanging sheet method, and the specific test conditions are as follows:
corrosion water: preparing water by adopting the standard in GB/T18175-2014;
test piece: the test piece specified in SH/T0085 and 1991 engine coolant corrosion determination method (glassware method) is adopted;
detecting the temperature: 89 ℃, time: 237 h. The specific experimental results are shown in table 2.
TABLE 2 results of the experiment
Note: the solder is the solder in SH/T0085-1991, and the aluminum is the cast aluminum in SH/T0085-1991.
The data in the table show that the sealant provided by the invention has an anti-corrosion effect on metal, and the ammonium citrate can play a role of a pH buffering agent, so that the strong acidic substances such as citric acid and the like can be effectively prevented from pitting corrosion on the reticular film formed by the organic dibasic acid and the alcohol amine compound.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (10)
1. The sealant is characterized by comprising the following raw materials in parts by weight:
30-45 parts of organic dibasic acid, 18-31 parts of alcohol amine compound, 5-15 parts of ammonium citrate and 20-30 parts of deionized water.
2. The occlusive agent according to claim 1, wherein said organic diacid is sebacic and/or adipic acid;
the alcohol amine compound is triethanolamine and/or ethanolamine.
3. The occlusive agent according to claim 1 or 2, wherein the occlusive agent comprises the following raw materials in parts by weight:
20-25 parts of sebacic acid, 10-20 parts of adipic acid, 15-25 parts of triethanolamine, 3-6 parts of ethanolamine, 5-15 parts of ammonium citrate and 20-30 parts of deionized water.
4. A method for preparing a occlusive agent, comprising the steps of:
and (3) uniformly mixing deionized water and ammonium citrate, sequentially adding organic dibasic acid and an alcohol amine compound, and stirring to obtain the closer.
5. The method according to claim 4, wherein the organic dibasic acid is added at a temperature of 75 to 85 ℃.
6. The process according to claim 4 or 5, wherein the organic dibasic acid is added, the temperature is raised to 85 to 90 ℃, and the alcohol amine compound is added after stirring for 25 to 35 min.
7. The process according to any one of claims 4 to 6, wherein the temperature of addition of the alkanolamine compound is 90 to 97 ℃.
8. The method as claimed in any one of claims 4-7, wherein the alkanolamine compound is added, and then stirred for 55-65 min, cooled to 85-90 ℃, stirred for 350-370 min, and then naturally cooled to room temperature.
9. The method according to any one of claims 4-8, wherein when there is more than one alcohol amine compound, the alcohol amine compounds are added separately and at an interval of 110-130 min.
10. Use of a occlusive agent as claimed in any of claims 1 to 3 or of a occlusive agent obtainable by a process for the preparation of a occlusive agent as claimed in any of claims 4 to 9 in a water circulation system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010482646.3A CN111809186A (en) | 2020-05-29 | 2020-05-29 | Closing agent and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010482646.3A CN111809186A (en) | 2020-05-29 | 2020-05-29 | Closing agent and preparation method and application thereof |
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| CN111809186A true CN111809186A (en) | 2020-10-23 |
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| CN202010482646.3A Pending CN111809186A (en) | 2020-05-29 | 2020-05-29 | Closing agent and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115537817A (en) * | 2022-10-24 | 2022-12-30 | 浙江康星科技有限公司 | Environment-friendly water-based antirust agent and preparation method and application thereof |
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| CN103305853A (en) * | 2012-03-09 | 2013-09-18 | 中国石油化工股份有限公司 | Cleaning agent for automobile cooling system |
| EP2888387A1 (en) * | 2012-08-22 | 2015-07-01 | Invista Technologies S.a r.l. | Aliphatic dicarboxylic acid mixture formulation |
| CN105463472A (en) * | 2015-12-08 | 2016-04-06 | 彭国泉 | Water-soluble antirust agent |
| CN107164060A (en) * | 2017-06-30 | 2017-09-15 | 合肥博创机械制造有限公司 | A kind of preparation method of rust remover for plant equipment |
| CN110055541A (en) * | 2019-05-08 | 2019-07-26 | 北京欧源化工环保科技有限公司 | A kind of water circulation system protective agent and its preparation process |
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2020
- 2020-05-29 CN CN202010482646.3A patent/CN111809186A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305853A (en) * | 2012-03-09 | 2013-09-18 | 中国石油化工股份有限公司 | Cleaning agent for automobile cooling system |
| EP2888387A1 (en) * | 2012-08-22 | 2015-07-01 | Invista Technologies S.a r.l. | Aliphatic dicarboxylic acid mixture formulation |
| CN105463472A (en) * | 2015-12-08 | 2016-04-06 | 彭国泉 | Water-soluble antirust agent |
| CN107164060A (en) * | 2017-06-30 | 2017-09-15 | 合肥博创机械制造有限公司 | A kind of preparation method of rust remover for plant equipment |
| CN110055541A (en) * | 2019-05-08 | 2019-07-26 | 北京欧源化工环保科技有限公司 | A kind of water circulation system protective agent and its preparation process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115537817A (en) * | 2022-10-24 | 2022-12-30 | 浙江康星科技有限公司 | Environment-friendly water-based antirust agent and preparation method and application thereof |
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