A water seal cleaning agent and its preparation method and application

Abstract

The present invention proposes a water seal unblocking cleaning agent and a preparation method and application thereof, belonging to the technical field of cleaning agents. The cleaning agent is prepared from the following raw materials by weight: 100-120 parts of water, 5-7 parts of antibacterial surfactant, 20-40 parts of n-hexanol, 3-5 parts of composite surfactant, 2-4 parts of citric acid, and 1-2 parts of disodium EDTA. The water seal unblocking cleaning agent prepared by the present invention has high antibacterial and antibacterial performance, strong detergency, high descaling rate, low metal corrosion, can effectively dissolve and clean the dirt on the water seal pipeline, and has broad application prospects.

Description

Technical Field

[0001] The invention relates to the technical field of cleaning agents, and in particular to a water seal unblocking cleaning agent and a preparation method and application thereof. Background Art

[0002] A water seal refers to a water column of a certain height in a device to prevent gas from entering the room from the drainage system. In building drainage pipes, a water seal refers to a water column of a certain height located under the drain outlet of sanitary appliances to resist changes in air pressure differences in the drain pipe and prevent gas from entering the room from the drainage system. This is usually achieved with a trap. Due to the movement of the body of a high-speed train, a water seal is needed to stabilize the water pressure and prevent the spread of odors. After long-term use, the water seal is prone to clogging and needs to be cleaned with a cleaning agent.

[0003] The existing cleaning agents used to produce high-speed train water seals have insufficient cleaning capacity and cannot quickly and efficiently dissolve and clean the dirt on the water seal pipes. As a result, dirt accumulates in the pipes over the years, which easily causes blockage and affects the normal operation of the pipes. At the same time, bacteria are also easily bred during the water seal process, so the cleaning agent is required to have certain bactericidal and antibacterial properties. Summary of the invention

[0004] The purpose of the present invention is to provide a water seal cleaning agent and its preparation method and application, which has high antibacterial and antimicrobial properties, strong detergency, high scale removal rate, and low metal corrosion. It can effectively dissolve and clean the dirt on the water seal pipe and has broad application prospects.

[0005] The technical solution of the present invention is achieved in this way:

[0006] The present invention provides a water seal unblocking cleaning agent, which is prepared from the following raw materials in parts by weight: 100-120 parts of water, 5-7 parts of antibacterial surfactant, 20-40 parts of n-hexanol, 3-5 parts of composite surfactant, 2-4 parts of citric acid, and 1-2 parts of disodium EDTA; the structural formula of the antibacterial surfactant is shown in Formula I:

[0007]

[0008] Wherein, R=C6-C8, C10 alkyl chain.

[0009] As a further improvement of the present invention, the preparation method of the antibacterial surfactant is as follows:

[0010] S1. Mix cyanuric chloride with borneol and alkali, heat and stir to react, recrystallize, filter, wash and dry to obtain intermediate 1, the structure of which is as follows:

[0011] S2. The intermediate 1 is mixed with a methylalkylamine and a base, heated and stirred for reaction, recrystallized, filtered, washed, and dried to obtain the intermediate 2, the structure of which is as follows: Wherein, R = C6-C8, C10 alkyl chain;

[0012] S3. The intermediate 2 is reacted with butane sultone to obtain the product.

[0013] As a further improvement of the present invention, the molar ratio of cyanuric chloride, borneol and base in step S1 is 1:0.9-1:3-5, the base is selected from at least one of triethylamine, diethylamine and ethylenediamine, and the temperature of the heating and stirring reaction is 50-60°C and the time is 2-4h.

[0014] As a further improvement of the present invention, the molar ratio of the intermediate 1, the alkylamine and the base in step S2 is 1:1.9-2:5-7, the base is selected from at least one of sodium carbonate, sodium bicarbonate, potassium carbonate and potassium bicarbonate, the methylalkylamine is selected from at least one of N-methylhexylamine, N-methylheptylamine, N-methyloctylamine and N-methyldecylamine, and the temperature of the heating and stirring reaction is 45-55°C and the time is 2-4h.

[0015] As a further improvement of the present invention, the molar ratio of the intermediate 2 to butanesultone in step S3 is 1:2-2.1, the reaction temperature is 45-55° C., and the reaction time is 20-24 h.

[0016] As a further improvement of the present invention, the preparation method of the antibacterial surfactant is as follows:

[0017] S1. 1 molar equivalent of cyanuric chloride, 0.9-1 molar equivalent of borneol, and 3-5 molar equivalent of a base are mixed and added to acetonitrile, heated to 50-60° C., stirred for reaction for 2-4 hours, and acetone is added for recrystallization, filtered, washed, and dried to obtain intermediate 1;

[0018] S2. 1 molar equivalent of intermediate 1, 1.9-2 molar equivalents of methylalkylamine and 5-7 molar equivalents of base were mixed and added to acetonitrile, heated to 45-55°C, stirred for 2-4h, and recrystallized by adding acetone, filtered, washed and dried to obtain intermediate 2;

[0019] S3. Add 1 molar equivalent of intermediate 2 and 2-2.1 molar equivalents of butane sultone to acetone, heat to 45-55°C, stir to react for 20-24h, filter, wash, and dry to obtain the product.

[0020] As a further improvement of the present invention, the composite surfactant includes a hydrophilic surfactant and a lipophilic surfactant in a mass ratio of 3-5:10-12, the hydrophilic surfactant is selected from at least one of Tween-20, Tween-40, Tween-60, Tween-80, and Tween-85, and the lipophilic surfactant is selected from at least one of Span-20, Span-40, Span-60, Span-80, and Span-85.

[0021] The present invention further protects a method for preparing the above-mentioned water seal unblocking cleaning agent, comprising the following steps: dissolving an antibacterial surfactant and a composite surfactant in water, adding citric acid and disodium EDTA, heating and stirring, adding n-hexanol, stirring and mixing evenly, to obtain the water seal unblocking cleaning agent.

[0022] As a further improvement of the present invention, the heating and stirring is performed at a temperature of 40-45° C. and for a time of 20-30 min.

[0023] The present invention further protects a use of the water seal unclogging cleaning agent in cleaning a water seal section drainage pipe.

[0024] The present invention has the following beneficial effects:

[0025] In the structure of cyanuric chloride, the s-triazine ring has a high stability. Since the nitrogen atom in the ring carries a pair of unbonded lone pairs of electrons and the electron cloud density of the carbon atom is low, it is easily attacked by power-donating groups such as -NH2, -OH, -SH and other functional groups to undergo nucleophilic substitution reactions. The resulting triazine ring derivatives have high antibacterial and antimicrobial activity.

[0026] Borneol, also known as borneol, has a high antibacterial effect, but it has the disadvantage of being volatile, which greatly limits its application. The present invention reacts cyanuric chloride with borneol, and the obtained product is further reacted with methyl alkylamine, and then reacted with butane sultone to obtain a quaternary ammonium salt structure product, which further improves the antibacterial and antimicrobial properties of the product. At the same time, the obtained product has high surface activity and improves the cleaning ability of stains.

[0027] The present invention also adds citric acid and disodium EDTA. The citric acid has strong acidity and a pH buffering effect and is less corrosive to metals. It is compounded with the antibacterial surfactant and disodium EDTA to remove calcium and magnesium scales, thereby greatly improving the scale removal rate.

[0028] The water seal unclogging cleaning agent prepared by the invention has high antibacterial and bacteriostatic performance, strong detergency, high descaling rate, low metal corrosion, can effectively dissolve and clean the dirt on the water seal pipeline, and has broad application prospects. DETAILED DESCRIPTION

[0029] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] Preparation Example 1 Preparation of antibacterial surfactant

[0031] Synthesis route:

[0032]

[0033] The specific method is as follows:

[0034] S1. 1mmol of cyanuric chloride, 0.9mmol of borneol and 3mmol of triethylamine were mixed and added into 100mL of acetonitrile, heated to 50°C, stirred for reaction for 2h, and then acetone was added for recrystallization, filtered, washed and dried to obtain intermediate 1; ESI-MS calculated value: C 13 H 18 Cl2N3O(M+H) + 302.07, found: 302.1, yield: 87%.

[0035] NMR results: 1 H NMR (300MHz, CDCl3) δ3.62 (t, 1H), 1.92 (m, 1H), 1.47-1.63 (m, 4H), 1.22-1.27 (m, 2H), 1.17 (s, 3H), 1.12 (s, 6H).

[0036] S2. 1 mmol of intermediate 1 was mixed with 1.9 mmol of N-methylhexylamine and 5 mmol of potassium carbonate and added to 100 mL of acetonitrile, heated to 45°C, stirred for 2 h, and then acetone was added for recrystallization, filtered, washed, and dried to obtain intermediate 2; ESI-MS calculated value: C 27 H 50 N5O(M+H) + 460.71, found: 460.7, yield: 84%.

[0037] NMR results: 1 H NMR (300MHz, CDCl3) δ3.65 (t, 1H), 3.02 (t, 4H), 2.49 (s, 6H), 1.94 (m, 1H), 1. 47-1.63(m, 4H), 1.22-1.33(m, 18H), 1.17(s, 3H), 1.10(s, 6H), 0.97(t, 6H).

[0038] S3. Add 1 mmol of intermediate 2 and 2 mmol of butane sultone into 50 mL of acetone, heat to 45°C, stir and react for 20 h, filter, wash and dry to obtain the product. ESI-MS calculated value: C 35 H 66 N5O7S2(M+H) + 732.43, found: 732.4, yield: 67%.

[0039] NMR results: 1 H NMR (300MHz, CDCl3) δ3.64 (t, 1H), 3.42 (t, 4H), 3.27 (m, 8H), 2.90 (s, 6H), 1.94 (m, 1H), 1. 72(m, 8H), 1.47-1.63(m, 4H), 1.22-1.33(m, 18H), 1.17(s, 3H), 1.10(s, 6H), 0.97(t, 6H).

[0040] Preparation Example 2 Preparation of antibacterial surfactant

[0041] The specific method is as follows:

[0042] S1. 1 mmol of cyanuric chloride, 1 mmol of borneol and 5 mmol of diethylamine were mixed and added into 100 mL of acetonitrile, heated to 60°C, stirred for 4 h, and then acetone was added for recrystallization, filtered, washed and dried to obtain intermediate 1;

[0043] S2. 1 mmol of intermediate 1 was mixed with 2 mmol of N-methylheptylamine and 7 mmol of sodium bicarbonate and added to 100 mL of acetonitrile, heated to 55°C, stirred for 4 h, and then acetone was added for recrystallization, filtered, washed, and dried to obtain intermediate 2; ESI-MS calculated value: C 29 H 54 N5O(M+H) + 488.76, found: 488.8, yield: 81%.

[0044] NMR results: 1 H NMR (300MHz, CDCl3) δ3.65 (t, 1H), 3.02 (t, 4H), 2.49 (s, 6H), 1.94 (m, 1H), 1. 47-1.63(m, 4H), 1.22-1.37(m, 22H), 1.17(s, 3H), 1.10(s, 6H), 0.97(t, 6H).

[0045] S3. Add 1 mmol of intermediate 2 and 2.1 mmol of butane sultone into 50 mL of acetone, heat to 55°C, stir and react for 24 h, filter, wash and dry to obtain the product. ESI-MS calculated value: C37 H 70 N5O7S2(M+H) + 760.46, found: 760.5, yield 60%.

[0046] NMR results: 1 H NMR (300MHz, CDCl3) δ3.65 (t, 1H), 3.41 (t, 4H), 3.27 (m, 8H), 2.90 (s, 6H), 1.94 (m, 1H), 1. 72(m, 8H), 1.47-1.63(m, 4H), 1.20-1.31(m, 22H), 1.16(s, 3H), 1.11(s, 6H), 0.96(t, 6H).

[0047] Preparation Example 3 Preparation of antibacterial surfactant

[0048] The specific method is as follows:

[0049] S1. 1 mmol of cyanuric chloride, 0.95 mmol of borneol and 4 mmol of triethylamine were mixed and added into 100 mL of acetonitrile, heated to 55°C, stirred for reaction for 3 h, and acetone was added for recrystallization, filtered, washed and dried to obtain intermediate 1;

[0050] S2. 1 mmol of intermediate 1 was mixed with 1.95 mmol of N-methyloctylamine and 6 mmol of sodium carbonate and added to 100 mL of acetonitrile, heated to 50°C, stirred for reaction for 3 h, and then acetone was added for recrystallization, filtered, washed, and dried to obtain intermediate 2; ESI-MS calculated value: C 31 H 58 N5O(M+H) + 516.46, found: 516.5, yield: 79%.

[0051] NMR results: 1 H NMR (300MHz, CDCl3) δ3.63 (t, 1H), 3.04 (t, 4H), 2.51 (s, 6H), 1.94 (m, 1H), 1. 47-1.61(m, 4H), 1.22-1.35(m, 26H), 1.15(s, 3H), 1.10(s, 6H), 0.98(t, 6H).

[0052] S3. Add 1 mmol of intermediate 2 and 2.05 mmol of butane sultone into 50 mL of acetone, heat to 50°C, stir and react for 22 h, filter, wash and dry to obtain the product. ESI-MS calculated value: C 39 H 74 N5O7S2(M+H) +789.16, found: 789.2, yield 58%.

[0053] NMR results: 1 H NMR (300MHz, CDCl3) δ3.62 (t, 1H), 3.45 (t, 4H), 3.25 (m, 8H), 2.92 (s, 6H), 1.91 (m, 1H), 1. 74(m, 8H), 1.44-1.60(m, 4H), 1.20-1.32(m, 26H), 1.15(s, 3H), 1.12(s, 6H), 0.94(t, 6H).

[0054] Test Example 1

[0055] The equilibrium surface tension of the aqueous solution of the antibacterial surfactant sample obtained in Preparation Examples 1-3 with different concentrations at (25±0.1)°C was tested by the platinum ring method, and each concentration was measured 5 times and the average value was taken. After the test, a γ-c curve was drawn with concentration (c) as the horizontal axis and surface tension (γ) as the vertical axis, and the cmc was determined according to the turning point of the curve, and the surface tension at this time was recorded. The results are shown in Table 1.

[0056] Table 1

[0057] Group <![CDATA[cmc(×10 -5 mol / L)]]> <![CDATA[γ cmc (mN / m)]]> Preparation Example 1 2.5 33.2 Preparation Example 2 2.2 32.9 Preparation Example 3 2.1 31.0

[0058] It can be seen from the above table that the antibacterial surfactants prepared in Preparation Examples 1-3 of the present invention have a lower critical micelle concentration and a lower surface tension at this time.

[0059] Example 1

[0060] This embodiment provides a water seal unclogging and cleaning agent.

[0061] The preparation method comprises the following steps: dissolving 5 g of the antibacterial surfactant prepared in Preparation Example 1 and 3 g of the composite surfactant in 100 mL of water, adding 2 g of citric acid and 1 g of disodium EDTA, heating to 40° C., stirring for 20 min, adding 20 g of n-hexanol, stirring and mixing for 20 min, and preparing a water seal unclogging cleaning agent.

[0062] The composite surfactant comprises Tween-20 and Span-20, with a mass ratio of 3:10.

[0063] Example 2

[0064] This embodiment provides a water seal unclogging and cleaning agent.

[0065] The preparation method comprises the following steps: dissolving 7 g of the antibacterial surfactant prepared in Preparation Example 2 and 5 g of the composite surfactant in 120 mL of water, adding 4 g of citric acid and 2 g of disodium EDTA, heating to 45° C., stirring for 30 min, adding 40 g of n-hexanol, stirring and mixing for 20 min, and preparing a water seal unclogging cleaning agent.

[0066] The complex surfactant includes Tween-40 and Span-40, with a mass ratio of 5:12.

[0067] Example 3

[0068] This embodiment provides a water seal unclogging and cleaning agent.

[0069] The preparation method comprises the following steps: dissolving 6 g of the antibacterial surfactant prepared in Preparation Example 3 and 4 g of the composite surfactant in 110 mL of water, adding 3 g of citric acid and 1.5 g of disodium EDTA, heating to 42° C., stirring for 25 min, adding 30 g of n-hexanol, stirring and mixing for 20 min, and preparing a water seal unclogging cleaning agent.

[0070] The composite surfactant comprises Tween-85 and Span-85, with a mass ratio of 4:11.

[0071] Comparative Example 1

[0072] Compared with Example 3, the difference is that no antibacterial surfactant is added.

[0073] This comparative example provides a water seal unclogging cleaning agent.

[0074] The preparation method comprises the following steps: dissolving 10 g of a composite surfactant in 110 mL of water, adding 3 g of citric acid and 1.5 g of disodium EDTA, heating to 42° C., stirring for 25 minutes, adding 30 g of n-hexanol, stirring and mixing for 20 minutes, and obtaining a water seal cleaning agent.

[0075] The composite surfactant comprises Tween-85 and Span-85, with a mass ratio of 4:11.

[0076] Comparative Example 2

[0077] Compared with Example 3, the difference is that no composite surfactant is added.

[0078] This comparative example provides a water seal unclogging cleaning agent.

[0079] The preparation method comprises the following steps: dissolving 10 g of the antibacterial surfactant prepared in Preparation Example 3 in 110 mL of water, adding 3 g of citric acid and 1.5 g of disodium EDTA, heating to 42° C., stirring for 25 min, adding 30 g of n-hexanol, stirring and mixing for 20 min, and preparing a water seal unclogging cleaning agent.

[0080] Comparative Example 3

[0081] Compared with Example 3, the difference is that no antibacterial surfactant and complex surfactant are added.

[0082] This comparative example provides a water seal unclogging cleaning agent.

[0083] The preparation method comprises the following steps: adding 3g of citric acid and 1.5g of disodium EDTA into 110mL of water, heating to 42°C, stirring for 25min, adding 30g of n-hexanol, stirring and mixing for 20min, and preparing a water seal unblocking cleaning agent.

[0084] Test Example 2

[0085] Take 10mL of 1wt% water seal cleaning agent prepared in Example 1-3 or Comparative Example 1-3 and an aqueous solution of similar products on the market and add them to a test tube of the same size. The same mass of simulated sewage pipe inner wall scale (0.5g red iron oxide + 0.2g aluminum hydroxide + 1g calcium carbonate) is added to the test tube. The actual cleaning effect of the cleaning force is judged by the time it takes for the scale to float up.

[0086] The results are shown in Table 2.

[0087] Table 2

[0088] Group Floating time (min) Example 1 37 Example 2 35 Example 3 32 Comparative Example 1 75 Comparative Example 2 83 Comparative Example 3 270 Commercially available 102

[0089] It can be seen from the above table that the water seal cleaning agent prepared in Examples 1-3 of the present invention has a good cleaning effect on scale.

[0090] Test Example 3

[0091] Foaming test: The Roche foam meter was set to 25°C, and the water seal cleaning agent prepared in Examples 1-3 of the present invention or Comparative Examples 1-3 and similar commercial products (prepared into a 5wt% aqueous solution) were placed at the bottom of the foam meter, and the scale was aligned to 50mL. A 200mL quantitative funnel was used to absorb the test solution, the center position of the funnel was fixed, the test solution was placed, and the foam height (mm) was recorded, retaining the integer.

[0092] Stable foam test: The Roche foam meter was set to 25°C, and the water seal cleaning agent prepared in Examples 1-3 of the present invention or Comparative Examples 1-3 and similar commercial products (prepared into a 5wt% aqueous solution) were placed at the bottom of the foam meter, and the scale was aligned to 50mL. A 200mL quantitative funnel was used to absorb the test solution, and the center position of the funnel was fixed. The test solution was placed, and the foam height (mm) after 30min was recorded, and the integer was retained.

[0093] The results are shown in Table 3.

[0094] Table 3

[0095] Group Foam height (mm) Foam height after 30 minutes (mm) Example 1 220 203 Example 2 215 200 Example 3 227 209 Comparative Example 1 170 102 Comparative Example 2 145 74 Comparative Example 3 10 0 Commercially available 125 31

[0096] It can be seen from the above table that the water seal unclogging cleaning agent prepared in Examples 1-3 of the present invention has good foaming and foam stability.

[0097] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A water seal cleaning agent, characterized in that: The invention is prepared from the following raw materials in parts by weight: 100-120 parts of water, 5-7 parts of antibacterial surfactant, 20-40 parts of n-hexanol, 3-5 parts of composite surfactant, 2-4 parts of citric acid and 1-2 parts of disodium EDTA; the composite surfactant comprises a hydrophilic surfactant and a lipophilic surfactant in a mass ratio of 3-5:10-12, the hydrophilic surfactant is selected from at least one of Tween-20, Tween-40, Tween-60, Tween-80 and Tween-85, and the lipophilic surfactant is selected from at least one of Span-20, Span-40, Span-60, Span-80 and Span-85; the structural formula of the antibacterial surfactant is as shown in Formula I: Formula I; Among them, R = C6-C8, C10 alkyl chain.

2. The water seal cleaning agent according to claim 1, characterized in that: The preparation method of the antibacterial surfactant is as follows: S1. Mix cyanuric chloride with borneol and alkali, heat and stir to react, recrystallize, filter, wash and dry to obtain intermediate 1, the structure of which is as follows: ; S2. The intermediate 1 is mixed with a methylalkylamine and a base, heated and stirred for reaction, recrystallized, filtered, washed, and dried to obtain the intermediate 2, the structure of which is as follows: , wherein R = C6-C8, C10 alkyl chain; S3. The intermediate 2 is reacted with butane sultone to obtain the product.

3. The water seal cleaning agent according to claim 2, characterized in that: In step S1, the molar ratio of cyanuric chloride, borneol and base is 1:0.9-1:3-5, the base is selected from at least one of triethylamine, diethylamine and ethylenediamine, the temperature of the heating and stirring reaction is 50-60° C., and the time is 2-4 hours.

4. The water seal cleaning agent according to claim 2, characterized in that: In step S2, the molar ratio of the intermediate 1, the alkylamine and the base is 1:1.9-2:5-7, the base is selected from at least one of sodium carbonate, sodium bicarbonate, potassium carbonate and potassium bicarbonate, the methylalkylamine is selected from at least one of N-methylhexylamine, N-methylheptylamine, N-methyloctylamine and N-methyldecylamine, and the temperature of the heating and stirring reaction is 45-55°C for 2-4h.

5. The water seal cleaning agent according to claim 2, characterized in that: In step S3, the molar ratio of the intermediate 2 to butanesultone is 1:2-2.1, the reaction temperature is 45-55° C., and the reaction time is 20-24 h.

6. The water seal cleaning agent according to claim 2, characterized in that: The preparation method of the antibacterial surfactant is as follows: S1. 1 molar equivalent of cyanuric chloride, 0.9-1 molar equivalent of dextroborneol and 3-5 molar equivalent of base are mixed and added to acetonitrile, heated to 50-60°C, stirred for reaction for 2-4h, and acetone is added for recrystallization, filtered, washed and dried to obtain intermediate 1; S2. 1 molar equivalent of intermediate 1, 1.9-2 molar equivalents of methylalkylamine and 5-7 molar equivalents of base are mixed and added to acetonitrile, heated to 45-55°C, stirred for reaction for 2-4h, and acetone is added for recrystallization, filtered, washed and dried to obtain intermediate 2; S3. Add 1 molar equivalent of intermediate 2 and 2-2.1 molar equivalents of butane sultone into acetone, heat to 45-55°C, stir to react for 20-24h, filter, wash and dry to obtain the product.

7. A method for preparing the water seal cleaning agent according to any one of claims 1 to 6, characterized in that: The method comprises the following steps: dissolving an antibacterial surfactant and a composite surfactant in water, adding citric acid and disodium EDTA, heating and stirring, adding n-hexanol, stirring and mixing evenly, and preparing a water seal unblocking cleaning agent.

8. The preparation method according to claim 7, characterized in that: The heating and stirring is performed at a temperature of 40-45°C and for a time of 20-30 minutes.

9. Use of the water seal cleaning agent as claimed in any one of claims 1 to 6 in cleaning water seal section drainage pipes.

Images