A neutralizing regulator and a method for preparing neutral chlorinated paraffin using the neutralizing regulator and application thereof
Patent Information
- Application Number
- CN202610958166.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-06-30
- Publication Date
- 2026-10-09
AI Technical Summary
[0006]本发明要解决的技术问题是:为了克服现有中和调剂调整后的氯化石蜡产品仍然导致金属加工液pH下降、工件锈蚀、配方不稳定的缺陷,本发明采取以下技术方案:
[0038] 1. The chlorinated paraffin prepared by this invention achieves a truly neutral pH: through the action of amide neutralizing agents, the pH of the chlorinated paraffin is precisely adjusted from 4.0–6.0 to 7.0–7.5 (see appendix for details). Figure 1 This completely solves the problem of acidic chlorinated paraffin lowering the pH of metalworking fluids.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of lubricating oil additive technology, specifically relating to a neutralizing agent and its method for preparing neutral chlorinated paraffin using the neutralizing agent, as well as its application. The neutral chlorinated paraffin prepared by this invention has a neutral pH value and can be used as an extreme pressure anti-wear agent in metalworking fluids, lubricating oils, rust-preventive oils, and other fields. Background Technology
[0002] Chlorinated paraffins are chlorinated derivatives of alkanes, classified into three main categories based on carbon chain length: short-chain (C10-C13), medium-chain (C14-C17), and long-chain (C18-C30). Medium- and long-chain chlorinated paraffins are used as lubricant additives, typically with a chlorine content of 30-70%. Chlorinated paraffins are a classic extreme pressure anti-wear agent, widely used in metalworking oils, gear oils, and stamping and drawing oils. Their mechanism of action involves the decomposition of chlorinated paraffins under high temperature and pressure conditions (approximately 200-400℃), releasing active chlorine which reacts with the metal surface to form a FeCl2 / FeCl3 protective film. This film exhibits low shear strength, effectively reducing the coefficient of friction and protecting the metal surface.
[0003] In the industrial production of chlorinated paraffin, due to the characteristics of the chlorination reaction mechanism, a certain amount of hydrogen chloride (HCl) inevitably remains in the product, resulting in an acidic finished product with a pH value typically between 4.0 and 6.0, and an acid value of approximately 0.2-2.0 mgKOH / g. The main serious problems associated with this acidic chlorinated paraffin in lubricant applications are: 1) Affecting the pH value of metalworking fluids: Metalworking fluids (especially water-based cutting fluids) need to maintain a certain pH range (8.5-9.5 is the optimal range for rust prevention) during use to inhibit bacterial growth and maintain rust prevention performance. When acidic chlorinated paraffin is added to the metalworking fluid formulation, it continuously releases HCl, gradually lowering the overall pH value, leading to workpiece corrosion and a significant reduction in cutting fluid life. 2) Exacerbating metal corrosion: The acidic environment accelerates the electrochemical corrosion process of metals. Even with the addition of rust inhibitors to the formulation, additional alkali is required to neutralize the HCl released by the acidic chlorinated paraffin, increasing formulation costs and causing unstable rust prevention effects. 3) Decreased formulation stability: In order to neutralize acidic chlorinated paraffin, rust inhibitors and pH adjusters need to be added to the formulation, which increases the complexity and instability of the formulation and may lead to problems such as product layering and precipitation. (4) Autocatalytic decomposition problem: Chlorinated paraffin will continue to slowly decompose and release HCl during storage and use. HCl itself catalyzes the further decomposition of chlorinated paraffin (autocatalytic reaction), causing the product acid value to increase and the color to darken over time, forming a vicious cycle.
[0004] To address the acidity issue of chlorinated paraffin, researchers in this field have attempted various neutralization methods, but all have significant drawbacks: 1) High-alkalinity calcium petroleum sulfonate neutralization: Calcium petroleum sulfonate has a high alkalinity, theoretically capable of neutralizing acidic substances in chlorinated paraffin. However, in practice, chlorinated paraffin neutralized with high-alkalinity calcium petroleum sulfonate exhibits significant yellowing and turbidity, affecting product appearance and transparency, making it unsuitable for metalworking fluids requiring clear product appearance. 2) Amine neutralizing agents such as TEA / DEA: Amine compounds such as triethanolamine (TEA) and diethanolamine (DEA) are alkaline and can be used for pH adjustment. However, chlorinated paraffin treated with these amine neutralizing agents also exhibits yellowing and turbidity, and the product has a distinct amine odor, making it unacceptable to downstream customers. 3) MDEA+DMF+oil-soluble azole composite solution: This solution uses methyl diethanolamine (MDEA) as the main neutralizing agent, supplemented with N,N-dimethylformamide (DMF) and oil-soluble azole compounds. In the short term, the product transparency is acceptable, but in terms of long-term stability, this approach has fundamental flaws: the MDEA·HCl salt produced by the reaction of MDEA and HCl has low solubility in the chlorinated paraffin system and will crystallize and precipitate after long-term storage; chlorinated paraffin continuously produces trace amounts of HCl during use, leading to the continuous accumulation of MDEA·HCl salt; oil-soluble azole compounds are inherently acidic and will consume some of the neutralizing agent's alkali content; the two amine salts (MDEA·HCl and DMF-related salts) may co-crystallize, accelerating turbidity; DMF is hygroscopic, and absorbing moisture from the air will accelerate the precipitation of amine salts. 4) Epoxy fatty acid methyl ester (EFAME) approach: Epoxy fatty acid methyl esters can react with HCl to produce hydroxy esters, theoretically consuming some acidic substances. However, in practice, adding a small amount (below 0.5%) has an insignificant effect on HCl capture by chlorinated paraffin and cannot adjust the pH of chlorinated paraffin to the true neutral range (7.0-7.5); adding a large proportion will significantly increase product costs and affect the extreme pressure performance of chlorinated paraffin.
[0005] Given the various shortcomings of existing chlorinated paraffin technologies, there is an urgent need in the field to develop a neutral chlorinated paraffin with a truly neutral pH (7.0-7.5), which is stable during long-term storage, does not become cloudy, does not change color, does not precipitate, has no odor, is compatible with metalworking fluid systems, does not affect the overall pH, has reasonable production costs, and is suitable for large-scale industrial applications. Summary of the Invention
[0006] The technical problem this invention aims to solve is: to overcome the shortcomings of existing chlorinated paraffin products, which, even after neutralization and adjustment, still cause a decrease in the pH of the metalworking fluid, workpiece corrosion, and unstable formulation. This invention adopts the following technical solution:
[0007] On one hand, the present invention provides a neutralizing regulator for preparing neutral chlorinated paraffin, wherein the neutralizing regulator is composed of oleamide compounds and cocoyl diethanolamide compounds.
[0008] According to the above-mentioned neutralizing regulator, the amount of the oleamide compound added accounts for 0.5 to 3.0% of the mass of chlorinated paraffin; the amount of the cocoyl diethanolamide compound added accounts for 0.3 to 2.0% of the mass of chlorinated paraffin.
[0009] According to the above-mentioned neutralizing regulator, the amount of the oleamide compound added accounts for 1.0 to 2.5% of the mass of chlorinated paraffin; the amount of the cocoyl diethanolamide compound added accounts for 0.5% to 1.8% of the mass of chlorinated paraffin.
[0010] According to the above-mentioned neutralizing regulator, the oleamide compound is at least one of oleic acid amide, erucic acid amide, cocoyl monoethanolamide and oleic acid diethanolamide; the cocoyl diethanolamide compound is at least one of 1:1 cocoyl diethanolamide, 1:2 cocoyl diethanolamide and cocoyl monoethanolamide.
[0011] According to the above-mentioned neutralizing regulator, the base value of the oleamide compound is 40-55 mgKOH / g; the base value of the cocoyl diethanolamide compound is 25-45 mgKOH / g.
[0012] On the other hand, a method for preparing neutral chlorinated paraffin using the above-mentioned neutralizing regulator is provided, comprising the following steps:
[0013] 1) Weigh the raw material chlorinated paraffin;
[0014] 2) Add the neutralizing regulator to the raw material chlorinated paraffin to carry out the neutralization reaction;
[0015] 3) The mixture after the neutralization reaction is aged to obtain a neutral chlorinated paraffin product.
[0016] According to the above method for preparing neutral chlorinated paraffin, the pH value of the raw material chlorinated paraffin in step 1) is 4.0 to 6.0, and the acid value is ≤2.0 mgKOH / g.
[0017] According to the above method for preparing neutral chlorinated paraffin, the neutralization reaction in step 2) is carried out under stirring conditions, with the stirring speed controlled at 200-500 r / min, the reaction temperature at 40-80℃, and the reaction time at 30-90 min; the aging treatment in step 3) is controlled at 40-60℃ and for 12-24 hours.
[0018] The neutral chlorinated paraffin of this invention is prepared by the above-described preparation method.
[0019] The present invention relates to the application of neutral chlorinated paraffin in lubricating oils, specifically in metalworking fluids, gear oils, cutting oils, stamping and drawing oils, rust-preventive oils, or extreme pressure lubricating oils.
[0020] When the neutral chlorinated paraffin of the present invention is used in lubricating oil, the amount of neutral chlorinated paraffin added accounts for 5 to 15% of the total mass of the lubricating oil formulation.
[0021] The chlorinated paraffin raw material used in this invention is heavy chlorinated paraffin with a density of 0.975–1.26 g / cm³ and a chlorine content of 20–52%; specifically selected from at least one of the following types:
[0022] 1) Light load type: density 0.975~0.995 g / cm³, chlorine content 20~26%;
[0023] 2) Medium-load type: density 1.06~1.10 g / cm³, chlorine content 31~35%;
[0024] 3) Heavy-duty type: density 1.11~1.26 g / cm³, chlorine content 36~52%.
[0025] This invention is the first to use a combination of two amide compounds as a neutralizing regulator. By utilizing the neutralization reaction between the amide compounds and HCl, the pH value of chlorinated paraffin is adjusted from 4.0 to 6.0 to the neutral range of 7.0 to 7.5.
[0026] When this invention uses a combination of two amide compounds as a neutralizing regulator, the amount of the oleamide compound added accounts for 1.5% of the mass of chlorinated paraffin; the amount of the cocoyl diethanolamide compound added accounts for 1.0% of the mass of chlorinated paraffin; or, the amount of the amide compound added accounts for 2.5% of the mass of chlorinated paraffin; the amount of the cocoyl diethanolamide compound added accounts for 1.8% of the mass of chlorinated paraffin.
[0027] Advantages of amide compounds as neutralizing agents:
[0028] 1) Moderate alkalinity: Amide compounds have a pH value in the range of 9.0-10.5, and will not cause product discoloration due to excessive alkalinity;
[0029] 2) Good oil solubility: Amide compounds have good oil solubility and good compatibility with chlorinated paraffin systems;
[0030] 3) Synergistic lubrication: Amide compounds themselves have certain lubricating properties, which can improve the lubrication performance of chlorinated paraffins;
[0031] 4) Rust prevention synergy: The polar groups of amide compounds can form a protective film on the metal surface, enhancing the rust prevention effect;
[0032] 5) No amine odor: Unlike small molecule amines such as TEA and DEA, amide compounds have low volatility and no obvious amine odor;
[0033] 6) Good stability: The amide hydrochloride formed by the reaction of amide and HCl has good solubility in the oil phase and is not easy to precipitate.
[0034] In the neutralizing agent of this invention, oleamide compounds serve as the main neutralizing agent with an alkalinity of 40–55 mgKOH / g, providing the primary alkaline neutralization capability and adjusting the pH of chlorinated paraffin to neutral. Cocoyl diethanolamide compounds serve as the auxiliary neutralizing agent with an alkalinity of 25–45 mgKOH / g, assisting in pH adjustment and enhancing the neutralization effect; improving the solubility and stability of the product in the oil phase; and providing additional lubricity and rust prevention.
[0035] Synergistic mechanism of the two amide compounds: The neutralizing regulator, oleamide, has a high base value and is responsible for the main neutralizing ability; the neutralizing regulator, cocoyl diethanolamide, although has a low base value, its alkanolamide structure enhances the solubility and dispersibility of amide hydrochloride in the oil phase, prevents the local aggregation and precipitation of neutralization products, and its hydrophilic-lipophilic balance improves the overall stability of the system.
[0036] When used in combination, the two amide compounds have a synergistic effect that makes the neutralization effect more stable and long-lasting. When used alone as a neutralizing regulator, oleamide compounds can achieve a neutral pH, slight turbidity may appear after long-term storage; when combined with cocoyl diethanolamide compounds as a neutralizing regulator, the product is clear, transparent, and stable over a long period of time.
[0037] The positive and beneficial effects of this invention are as follows:
[0038] 1. The chlorinated paraffin prepared by this invention achieves a truly neutral pH: through the action of amide neutralizing agents, the pH of the chlorinated paraffin is precisely adjusted from 4.0–6.0 to 7.0–7.5 (see appendix for details). Figure 1 This completely solves the problem of acidic chlorinated paraffin lowering the pH of metalworking fluids.
[0039] 2. The neutral chlorinated paraffin prepared by this invention does not lower the pH of the metalworking fluid: When the neutral chlorinated paraffin prepared by this invention is added to the metalworking fluid formula, since its pH is neutral, it will not consume the rust inhibitor and alkali in the formula, and the metalworking fluid can be stably maintained in the optimal rust prevention range (pH 8.5-9.5).
[0040] 3. The neutral chlorinated paraffin prepared by this invention is stable during long-term storage, without discoloration or turbidity: The amide hydrochloride formed by the neutralizing regulator amide compound and HCl in this invention has good solubility in the oil phase and will not crystallize out due to low solubility like MDEA·HCl. Therefore, after long-term storage tests, the neutral chlorinated paraffin prepared by this invention is clear and transparent in appearance, without turbidity, layering, or precipitation (see appendix for details). Figure 2 and attached Figure 3 ).
[0041] 4. The neutral chlorinated paraffin prepared by this invention has no obvious amine odor: The amide compounds used in this invention have a much lower volatility than small molecule amines (such as TEA and DEA), and the product has no obvious amine odor, which is highly accepted by downstream customers.
[0042] 5. The neutral chlorinated paraffin prepared by this invention has both rust-preventive and lubricating functions: Because the amide compounds used in this invention have polar groups, they can form a physical adsorption film on the metal surface, enhancing the rust-preventive performance of the product. Simultaneously, the presence of amide groups improves the boundary lubrication performance of the chlorinated paraffin.
[0043] 6. Synergistic effect of the two amides: Although oleamide compounds alone can neutralize to neutral pH, they may become slightly turbid during long-term storage; when combined with coconut oil diethanolamide compounds, their alkanolamide structure enhances the dispersibility of the amide salt in the oil phase, resulting in a clear, transparent product that is stable over a long period of time.
[0044] 7. Expanding application areas: The neutral chlorinated paraffin prepared by this invention can be used in mid-to-high-end metalworking fluid formulations that have high requirements for product appearance and pH stability, thus expanding the application scope of chlorinated paraffin in the field of lubricating oil.
[0045] The test results of relevant performance indicators of the neutral chlorinated paraffin prepared by this invention are detailed in Table 1.
[0046] Table 1. Test results of relevant properties of the neutral chlorinated paraffin of this invention.
[0047]
[0048] The neutral chlorinated paraffin products prepared by this invention are classified into the following three types according to their density and chlorine content (see Table 2 for details).
[0049] Table 2 Classification of Neutral Chlorinated Paraffin Products of the Present Invention
[0050] Attached Figure Description
[0051] Figure 1 A comparative chart of measured pH values of the neutral chlorinated paraffin prepared by this invention and existing acidic chlorinated paraffin;
[0052] Depend on Figure 1 Actual measurements show that ordinary chlorinated paraffin has a pH of 4.5, which is significantly acidic. This is due to residual HCl and the release of HCl from thermal decomposition during the production process. An acidic environment is a direct cause of metal corrosion (especially rusting of cast iron). The neutral chlorinated paraffin prepared by this invention using a neutralizing regulator has a pH value in the neutral range of 7.0 to 7.5, fundamentally eliminating the risk of acid corrosion.
[0053] Figure 2 Storage tests comparing neutral chlorinated paraffins prepared using the neutralizing agent of this invention and comparative neutralizing agents. Figure 1 ;
[0054] Figure 3 Storage tests comparing neutral chlorinated paraffins prepared using the neutralizing agent of this invention and comparative neutralizing agents. Figure 2 ;
[0055] Depend on Figure 2 and Figure 3 It is evident that different neutralizing agent formulations significantly affect the neutralization effect and long-term stability of chlorinated paraffin. The neutralizing regulator formulation of this invention can maintain the sample's clear and transparent appearance and stable pH neutrality during a 28-day storage period, demonstrating significant effectiveness.
[0056] Figure 4 Figure showing the rust-preventive performance test results of ordinary chlorinated paraffin after 72 hours of salt spray test.
[0057] Depend on Figure 4 It was found that ordinary chlorinated paraffin specimens showed severe corrosion after 72 hours of salt spray testing. Large areas of the specimen surface were covered with reddish-brown rust spots and dark brown corrosion marks, indicating significant erosion of the metal substrate. This is because the acidic environment (pH 4.5) of ordinary chlorinated paraffin continuously releases HCl, which, under the synergistic effect of salt spray (chloride ions), significantly accelerates metal corrosion.
[0058] Figure 5 The rust prevention performance test results of the neutral chlorinated paraffin prepared in Example 6 of this invention after 72 hours of salt spray test are shown in the figure.
[0059] Depend on Figure 5 It can be seen that the neutral chlorinated paraffin test piece prepared by this invention showed only a few scattered rust spots after 72 hours of salt spray testing, with the vast majority of the surface remaining smooth. The rust prevention effect is significantly better than that of ordinary chlorinated paraffin. The neutral environment eliminates the acid corrosion of metals by HCl, while the neutralization system has a certain protective film-forming effect on the metal surface, effectively inhibiting corrosion under salt spray conditions. Detailed Implementation
[0060] The present invention will be further illustrated below with reference to the embodiments, but this does not limit the scope of protection of the technical solution of the present invention.
[0061] Example 1:
[0062] The present invention is used to prepare a neutralizing regulator for neutral chlorinated paraffin. It is prepared by mixing 1.5 parts of oleic acid amide (neutralizing regulator A, with an alkalinity of about 48 mg KOH / g) and 1.0 part of 1:1 type cocoyl diethanolamide (neutralizing regulator B, with an alkalinity of about 35 mg KOH / g) evenly.
[0063] Example 2:
[0064] The detailed steps of the method for preparing neutral chlorinated paraffin using the neutralizing regulator described in Example 1 are as follows:
[0065] 1) The chlorinated paraffin raw material was tested and found to have a density of approximately 0.985 g / cm³, a pH value of 4.8, an acid value of approximately 0.2 mg KOH / g, indicating acidity, and a chlorine content of approximately 23%.
[0066] 2) The neutralizing regulator obtained in Example 1 was added to 100 parts of raw material chlorinated paraffin, and the neutralization reaction was carried out for 60 min under stirring conditions of 50°C and 300 r / min;
[0067] 3) Transfer the mixture after neutralization reaction to a maturation container and allow it to stand at 50°C for 18 hours to obtain a neutral chlorinated paraffin product.
[0068] The neutral chlorinated paraffin product prepared in this example was tested, and the test results are detailed in Table 3.
[0069] Table 3. Test results of the neutral chlorinated paraffin product prepared in Example 2
[0070]
[0071] Example 3:
[0072] The present invention is used to prepare a neutralizing regulator for neutral chlorinated paraffin. It is prepared by mixing 2.0 parts of oleic acid amide (neutralizing regulator A, with an alkalinity of about 47 mg KOH / g) and 1.5 parts of 1:1 type cocoyl diethanolamide (neutralizing regulator B, with an alkalinity of about 32 mg KOH / g) evenly.
[0073] Example 4:
[0074] The detailed steps of the method for preparing neutral chlorinated paraffin using the neutralizing regulator described in Example 3 are as follows:
[0075] 1) The chlorinated paraffin raw material was tested and found to have a density of approximately 1.08 g / cm³, a pH value of 5.0, an acid value of approximately 0.2 mg KOH / g, indicating acidity, and a chlorine content of approximately 33%.
[0076] 2) The neutralizing regulator obtained in Example 3 was added to 100 parts of raw material chlorinated paraffin, and the neutralization reaction was carried out at 60°C and 400 r / min for 75 min.
[0077] 3) Transfer the mixture after neutralization reaction to a curing container and let it stand at 55°C for 20 hours to obtain a neutral chlorinated paraffin product.
[0078] The neutral chlorinated paraffin product prepared in this example was tested, and the test results are detailed in Table 4.
[0079] Table 4. Test results of the neutral chlorinated paraffin product prepared in Example 4
[0080]
[0081] Example 5:
[0082] The present invention is used to prepare a neutralizing regulator for neutral chlorinated paraffin. It is prepared by mixing 2.5 parts of oleic acid diethanolamide (neutralizing regulator A, with an alkalinity of about 46 mg KOH / g) and 1.8 parts of 1:2 type coconut oil monoethanolamide (neutralizing regulator B, with an alkalinity of about 33 mg KOH / g) evenly.
[0083] Example 6:
[0084] The detailed steps of the method for preparing neutral chlorinated paraffin using the neutralizing regulator described in Example 5 are as follows:
[0085] 1) The chlorinated paraffin raw material was tested and found to have a density of approximately 1.13 g / cm³, a pH value of 4.6, an acid value of approximately 0.2 mg KOH / g, indicating acidity, and a chlorine content of approximately 38%.
[0086] 2) The neutralizing regulator obtained in Example 5 was added to 100 parts of raw material chlorinated paraffin, and the neutralization reaction was carried out at 70°C and 350 r / min for 90 min.
[0087] 3) Transfer the mixture after neutralization reaction to a curing container and let it stand at 60°C for 24 hours to obtain a neutral chlorinated paraffin product.
[0088] The neutral chlorinated paraffin product prepared in this example was tested, and the test results are detailed in Table 5.
[0089] Table 5. Test results of the neutral chlorinated paraffin product prepared in Example 6
[0090]
[0091] Example 7:
[0092] This invention relates to a neutralizing regulator for preparing neutral chlorinated paraffin, which is obtained by uniformly mixing 3.0 parts of oleic acid diethanolamide (neutralizing regulator A, with an alkalinity of about 48 mg KOH / g) and 2.0 parts of coconut oil monoethanolamide (neutralizing regulator B, with an alkalinity of about 33 mg KOH / g).
[0093] Example 8:
[0094] The detailed steps of the method for preparing neutral chlorinated paraffin using the neutralizing regulator described in Example 7 are as follows:
[0095] 1) The chlorinated paraffin raw material was tested and found to have a density of approximately 1.08 g / cm³, a pH value of 4.5, an acid value of approximately 0.2 mg KOH / g, indicating acidity, and a chlorine content of approximately 33%.
[0096] 2) The neutralizing regulator obtained in Example 7 was added to 100 parts of raw material chlorinated paraffin, and the neutralization reaction was carried out at 60°C and 400 r / min for 70 min.
[0097] 3) Transfer the mixture after neutralization reaction to a curing container and let it stand at 50°C for 20 hours to obtain a neutral chlorinated paraffin product.
[0098] The neutral chlorinated paraffin product prepared in this example was tested, and the test results are detailed in Table 6.
[0099] Table 6. Test results of the neutral chlorinated paraffin product prepared in Example 8
[0100]
[0101] Comparative test (28-day stability comparison of neutralizing regulator formulations in groups A, B, and C):
[0102] To verify the synergistic effect of the two amide compounding schemes of the present invention, the following control experiment was designed (see Table 7 for details).
[0103] Table 7. Neutralization regulator ratio in control experiment
[0104]
[0105] Note: The total amount of neutralizing agent added to groups B and C was the same as that in group A (4.3 parts) to control for variables.
[0106] Neutral chlorinated paraffin with a density of 1.13 g / cm³ and an acid value of approximately 0.2 mg KOH / g was prepared using the neutralizing agent formulation from the control experiment described above. The preparation method was the same as in Example 6.
[0107] The results of the control experiment are detailed in Table 8.
[0108] Table 8 Analysis of Control Experiment Results
[0109]
[0110] Samples were prepared on May 9, 2026, and observed for 17 days. All three groups remained clear and transparent (see attached). Figure 2 The observation was continued for 28 days, and the results are detailed in Table 9 and Appendix. Figure 3 .
[0111] Table 9. Analysis of the results of the control trial after 28 days
[0112]
[0113] The experimental analysis and comparison show that Group A of this invention performed best. After 28 days, the sample was nearly colorless and transparent, with a pH of 7.5, maintaining neutral stability without turbidity, precipitation, or foaming, indicating that the formulation had sufficient neutralization effect and good long-term stability. Group B performed moderately, showing a light yellow color, layering, and slight turbidity after 28 days. While the pH was 7.1, indicating neutrality, neutralization was not thorough, or some components precipitated. Group C performed the worst, with the color deepening to dark amber after 28 days, becoming nearly opaque, with white foam appearing on the surface. The pH was 6.2, significantly acidic, indicating insufficient neutralization capacity. Chlorinated paraffin continued to decompose, producing HCl, accompanied by oxidation, discoloration, and gas release. Therefore, different neutralizing agent formulations significantly affect the neutralization effect and long-term stability of chlorinated paraffin. The formulation in Group A maintained a clear and transparent appearance and a stable neutral pH during the 28-day storage period, making it the optimal solution.
[0114] Rust prevention application effect verification test:
[0115] The neutral chlorinated paraffin and acidic chlorinated paraffin (control group) prepared in Example 2 of this invention were respectively added to the metalworking fluid formulation for comparative testing. The test formulations and results are detailed in Tables 10 and 11. Figure 4-5 .
[0116] Table 10 Application Test Formulation
[0117]
[0118] Table 11 Application Test Results
[0119]
[0120] Test results show that the pH value of the metalworking fluid using the neutral chlorinated paraffin of this invention is stable in the optimal range for rust prevention (8.5-9.5), the workpiece is free from rust, and the service life of the cutting fluid is significantly extended.
[0121] Comparison of the rust-preventive properties of neutral chlorinated paraffin and ordinary chlorinated paraffin prepared by this invention in a 72-hour salt spray test (see attached results for details). Figure 4-5 ):
[0122] Depend on Figure 4 It was found that ordinary chlorinated paraffin test pieces showed severe corrosion after 72 hours of salt spray testing. Large areas of the test piece surface were covered with reddish-brown rust spots and dark brown corrosion marks, indicating significant erosion of the metal substrate. This is because the acidic environment of ordinary chlorinated paraffin (pH 4.5) continuously releases HCl, which, under the synergistic effect of salt spray (chloride ions), significantly accelerates metal corrosion.
[0123] Depend on Figure 5 It can be seen that the neutral chlorinated paraffin test piece prepared by this invention showed only a few scattered rust spots after 72 hours of salt spray testing, with the vast majority of the surface remaining smooth. The rust prevention effect is significantly better than that of ordinary chlorinated paraffin. The neutral environment eliminates the acid corrosion of metals by HCl, while the neutralization system has a certain protective film-forming effect on the metal surface, effectively inhibiting corrosion under salt spray conditions.
[0124] As can be seen from the above, the neutral chlorinated paraffin prepared by this invention exhibits a significantly different rust-preventive effect compared to ordinary chlorinated paraffin in the 72-hour salt spray test. Ordinary chlorinated paraffin samples showed severe corrosion, while neutral chlorinated paraffin samples showed only slight corrosion. This result directly proves that by adjusting the pH of the chlorinated paraffin from acidic (4.5) to neutral (7.0-7.5) in this invention, its rust-preventive protection ability for ferrous metals is fundamentally improved.
Claims
1. A neutralizing regulator for preparing neutral chlorinated paraffin, characterized in that: The neutralizing regulator is a compound of oleamide compounds and cocoyl diethanolamide compounds.
2. The neutralizing regulator according to claim 1, characterized in that: The amount of the oleamide compound added accounts for 0.5 to 3.0% of the mass of chlorinated paraffin; the amount of the cocoyl diethanolamide compound added accounts for 0.3 to 2.0% of the mass of chlorinated paraffin.
3. The neutralizing regulator according to claim 2, characterized in that: The amount of the oleamide compound added accounts for 1.0 to 2.5% of the mass of chlorinated paraffin; the amount of the cocoyl diethanolamide compound added accounts for 0.5% to 1.8% of the mass of chlorinated paraffin.
4. The neutralizing regulator according to claim 1 or 2, characterized in that: The oleamide compound is at least one of oleic acid amide, erucic acid amide, cocoyl monoethanolamide and oleic acid diethanolamide; the cocoyl diethanolamide compound is at least one of 1:1 cocoyl diethanolamide, 1:2 cocoyl diethanolamide and cocoyl monoethanolamide.
5. The neutralizing regulator according to claim 1 or 2, characterized in that: The oleamide compounds have an alkalinity of 40–55 mg KOH / g; the cocoyl diethanolamide compounds have an alkalinity of 25–45 mg KOH / g.
6. A method for preparing neutral chlorinated paraffin using the neutralizing regulator of claim 1, characterized in that, Includes the following steps: 1) Weigh the raw material chlorinated paraffin; 2) Add the neutralizing regulator to the raw material chlorinated paraffin to carry out the neutralization reaction; 3) The mixture after the neutralization reaction is aged to obtain a neutral chlorinated paraffin product.
7. The method for preparing neutral chlorinated paraffin according to claim 6, characterized in that: The pH value of the raw material chlorinated paraffin mentioned in step 1) is 4.0 to 6.0, and the acid value is ≤2.0 mgKOH / g.
8. The method for preparing neutral chlorinated paraffin according to claim 6, characterized in that: The neutralization reaction described in step 2) is carried out under stirring conditions, with the stirring speed controlled at 200-500 r / min, the reaction temperature at 40-80℃, and the reaction time at 30-90 min; the ripening treatment described in step 3) is carried out at a temperature controlled at 40-60℃ and for a time of 12-24 hours.
9. A neutral chlorinated paraffin, prepared by the preparation method described in claim 6.
10. The application of a neutral chlorinated paraffin in lubricating oil, characterized in that: It can be used in metalworking fluids, gear oils, cutting oils, stamping and drawing oils, rust-preventive oils, or extreme pressure lubricants.