A method for preparing an inorganic dust cleaning agent

Abstract

The present invention provides a method for preparing an inorganic dust cleaner, wherein a small molecule monomer with an amide group and a silane group undergoes an addition reaction with a macromolecular unsaturated polyether with a long chain structure under the action of an initiator through a low-temperature aqueous phase free radical polymerization reaction, thereby obtaining a polymer cleaner with a comb-shaped molecular structure. The inorganic powder particle agglomerates can be effectively adsorbed and dispersed, thereby removing stubborn dust on the "concave and convex surface", and the cleaning effect is good.

Description

Technical Field

[0001] The invention relates to the technical field of inorganic dust cleaning, and in particular to a method for preparing an inorganic dust cleaning agent. Background Art

[0002] In industrial parks with large amounts of dust and on both sides of roads, there is a problem of a lot of dust accumulation on houses and leaves of green plants. These dust accumulations are long-term and large-scale dust accumulations that form agglomerates and adhere to the surface of houses and leaves. Dust agglomerates are difficult to clean by mechanical washing. In particular, the dust accumulation on the leaves blocks the stomata on the leaf surface, affecting the photosynthesis of plants, causing the leaves to turn yellow or even wither. In addition, dust is also easy to accumulate on furniture and electrical appliances in the home. If the furniture and electrical appliances have smooth surfaces, the dust on the surface is easy to clean. However, for some furniture and electrical appliances with frosted surfaces, due to the uneven surface, when wiping with a wet towel, dust enters the gaps, resulting in gray stains on the furniture and electrical appliances after wiping, affecting the clean environment in the house.

[0003] The commonly used cleaning agents on the market currently rely mainly on the hydrophilic and lipophilic groups in the molecular structure of the surfactant to form a directional arrangement in the solution and clean the surface of the object under the action of external force, but they can only clean the oil stains on the surface and the dirt that is easier to wash off. As for the inorganic dust particle agglomerates on the surface of plants or furniture and electrical appliances, since there are no lipophilic groups, it is difficult to form a good adsorption with the surfactant molecules, so traditional surfactants cannot effectively clean the inorganic dust accumulation on the "bumpy surface". Therefore, how to clean the inorganic dust particle agglomerates on the "bumpy surface" has become a problem that needs to be solved urgently. Summary of the invention

[0004] In view of the above-mentioned deficiencies in the prior art, the present invention provides an inorganic dust cleaner, which is a polymer cleaner containing amide groups and silane groups on a comb-shaped molecular chain, which can effectively adsorb and disperse inorganic powder particle agglomerates, thereby removing stubborn dust accumulation on the "bumpy surface" and having a good cleaning effect.

[0005] The technical solution adopted to achieve the above-mentioned purpose of the present invention is:

[0006] A method for preparing an inorganic dust cleaning agent comprises the following steps: (1) preparing a base material: adding an unsaturated polyether monomer A and an oxidant into a reaction kettle, adding water to dissolve the monomers and stirring the mixture evenly;

[0007] (2) Solution ① Preparation: Weigh the thiol chain transfer agent and reducing agent, add water to dissolve and stir evenly;

[0008] (3) Preparation of solution ②: weigh unsaturated amide monomer B and unsaturated silane monomer C, add water to dissolve and stir evenly;

[0009] (4) The bottom material in the reaction kettle is heated to 35-55° C., and solutions ① and ② are added dropwise to the reaction kettle at the same time. The addition time is 1-4 hours, and the reaction temperature is controlled at 35-60° C. The total mass concentration of monomers A, B and C is controlled to be 30-60%. After the addition is completed, the reaction is kept warm for 1-2 hours, cooled to room temperature, an alkaline compound is added to adjust the pH to 6.5-7.5, and water is added to adjust the solid content to 20-30%, thereby obtaining an inorganic dust cleaner.

[0010] The molar ratio of the monomers A, B and C is 1:(2-9):(1-3).

[0011] The monomer A is a block polyether macromonomer, and its general formula is:

[0012]

[0013] In the above general formula, R 1 is H or methyl, R 2 is H or methyl, A is CH 2 or CH 2 CH 2 ; x is an integer from 10 to 50, and y is an integer from 10 to 150.

[0014] The monomer A is one or a mixture of any proportion of two or more of allyl alcohol, butenol, isobutenol or isopentenol with ethylene oxide and propylene oxide.

[0015] The monomer B is one or a mixture of two or more of N-vinyl caprolactam, N,N-dimethylacrylamide, N,N-diethylacrylamide, isopropylacrylamide, N-vinylpyrrolidone, N-vinylacetamide, N-vinylformamide, and N-methyl-N-vinylacetamide.

[0016] The monomer C is one or a mixture of two or more of γ-methacryloxypropyltrimethoxysilane, vinyltrimethoxysilane and vinyltriethoxysilane.

[0017] The oxidant is one of hydrogen peroxide, ammonium persulfate, potassium persulfate, tert-butyl hydroperoxide or isopropylbenzene hydroperoxide or a mixture of two of them in any proportion. The amount of the oxidant is 1-8% of the total molar number of the three monomers A, B and C.

[0018] The mercaptan chain transfer agent is one or a mixture of any proportion of mercaptoacetic acid, mercaptopropionic acid and mercaptoethanol, and the amount of the chain transfer agent is 1-15% of the total molar number of the three monomers A, B and C.

[0019] The reducing agent is one of vitamin C, Rongalite, sodium bisulfite or Mohr's salt, or a mixture of two or more of them in any proportion, and the amount of the reducing agent is 0.1-2% of the total molar number of the three monomers A, B and C; the alkaline compound is one of ammonia water and alkali metal hydroxide, or a mixture of two or more of them in any proportion.

[0020] The number average molecular weight of the prepared inorganic dust cleaning agent is 20000-80000.

[0021] Compared with the prior art, the technical solution of the present invention has the following advantages: (1) The inorganic dust cleaning agent of the present invention is based on the molecular structure design theory, and functional amide groups and silane groups are introduced into the unsaturated polyether to obtain a high molecular polymer with a comb-shaped molecular structure. After hydrolysis, the silane group can react with the hydroxyl groups on the surface of the inorganic dust particles to produce chemical adsorption, and the amide group can complex the ions in the liquid phase to form a gel, which plays a role in bridging different dust particles. The multifunctional groups on the main chain of the high molecular polymer with a comb-shaped molecular structure are widely distributed, and physical and chemical adsorption is produced on the surface of the dust agglomerates, which can greatly enhance the adsorption capacity of the polymer molecules on the inorganic powder particle agglomerates. At the same time, the steric hindrance of the long side chains of the polymer molecules can "break up" the powder particle agglomerates, making the agglomerates easy to be cleaned under the flushing of external forces, thereby effectively cleaning the stubborn inorganic dust particles on the "concave and convex surfaces" (such as leaf surfaces, frosted furniture and electrical appliance surfaces, etc.).

[0022] (2) The inorganic dust cleaning agent provided by the present invention is prepared by low-temperature initiated aqueous phase free radical polymerization reaction, which has simple technology, easy process control, low cost and easy industrial promotion and application.

[0023] (3) When the inorganic dust cleaner provided by the present invention is used to clean stubborn dust on the surfaces of exterior doors, tiles, furniture, blades, etc., the cleaning effect is good and the dust deposited in small gaps can be cleaned up. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 This is a diagram showing the cleaning effect of the inorganic dust cleaner provided in Example 1 and the cleaner purchased on the market when used for the exterior door;

[0025] Figure 2 The inorganic dust cleaner provided in Example 2 and the commercially available cleaner are used for cleaning effect diagrams of exterior wall tiles;

[0026] Figure 3 This is a diagram showing the cleaning effect of the inorganic dust cleaner provided in Example 3 and the commercially available cleaner on a metal surface;

[0027] Figure 4This is a diagram showing the cleaning effect of the inorganic dust cleaner provided in Example 4 and the commercially available cleaner on a desktop;

[0028] Figure 5 This is a diagram showing the cleaning effect of the inorganic dust cleaner provided in Example 4 and the commercially available cleaner on plant leaves; DETAILED DESCRIPTION

[0029] The following examples describe the preparation process of the inorganic dust cleaning agent of the present invention in more detail, and these examples are given in an illustrative manner so that technicians familiar with this project can understand the content of the present invention and implement it, but these examples do not limit the scope of protection of the present invention. All equivalent changes or modifications made according to the spirit and essence of the present invention should be included in the scope of protection of the present invention.

[0030] The unsaturated polyether monomers A in the embodiments of the present invention are all commercial products and can be purchased on the market.

[0031] In the embodiments of the present invention, the number average molecular weight of the copolymers was tested using a Viscotek TDA305max multi-detector gel permeation chromatograph produced by Malvern, UK, with a mobile phase of 0.1 mol / L sodium nitrate solution, a flow rate of 0.7 mL / min, and a chromatographic column of A-Guard+1x A6000M.

[0032] Example 1

[0033] The preparation method of the inorganic dust cleaning agent in this embodiment comprises the following steps: (1) preparation of base material: in a four-necked flask equipped with a thermometer and a stirrer, 320.96 g of methyl allyl polyoxyethylene-polyoxypropylene ether (0.08 mol), 1.186 g of 27.5% hydrogen peroxide and water are added and mixed, and stirred evenly;

[0034] (2) Solution ① Preparation: Weigh 1.017 g (0.0096 mol) of mercaptopropionic acid and 0.281 g (0.0016 mol) of vitamin C, add water to dissolve and stir evenly;

[0035] (3) Preparation of solution ②: Weigh 15.84 g (0.16 mol) of N,N-dimethylacrylamide and 19.84 g (0.08 mol) of γ-methacryloxypropyltrimethoxysilane, add water to dissolve and stir evenly;

[0036] (4) Heat the base material to 45° C. and simultaneously drip solutions ① and ② into the base material. Solution ① is dripped for 4 hours and solution ② is dripped for 3.5 hours. The total mass concentration of monomers A, B and C is controlled to be 35%. After the dripping is completed, keep the reaction warm for 1 hour, cool to room temperature, add sodium hydroxide solution, adjust the pH to 7, add water to adjust the solid content to 25% of a slightly yellow transparent liquid, and test its number average molecular weight to be 42,000.

[0037] The inorganic dust cleaning agent prepared in this example and the common cleaning agent purchased on the market (Comparative Example 1) were used to clean the dust on the outer door. The cleaning effect was as follows: Figure 1 The inorganic dust cleaner prepared in this embodiment can effectively clean the dust agglomeration particles on the outer door, and has a good cleaning effect. The outer door is clean and bright after cleaning, while the ordinary cleaner purchased can only clean the loose dust on the surface of the outer door, and it is still difficult to remove the stubborn dust.

[0038] Example 2

[0039] The preparation method of the inorganic dust cleaning agent in this embodiment comprises the following steps: (1) preparation of base material: in a four-necked flask equipped with a thermometer and a stirrer, 480 g of methyl butyl polyoxyethylene-polyoxypropylene ether (0.08 mol), 3.192 g (0.014 mol) of ammonium persulfate and water are added and mixed and stirred evenly;

[0040] (2) Solution ① Preparation: Weigh 1.747 g (0.0224 mol) of mercaptoethanol and 0.330 g (0.0028 mol) of Rongalite, add water to dissolve and stir evenly;

[0041] (3) Preparation of solution ②: Weigh 35.52 g (0.32 mol) of N-vinyl pyrrolidone and 11.84 g (0.08 mol) of vinyl trimethoxysilane, add water to dissolve and stir evenly;

[0042] (4) Heat the base material to 40° C. and simultaneously drip solutions ① and ② into the base material. Solution ① is dripped for 3.5 hours and solution ② is dripped for 3 hours. The total mass concentration of monomers A, B and C is controlled to be 30%. After the dripping is completed, keep the reaction warm for 1 hour, cool to room temperature, add potassium hydroxide solution, adjust the pH to 7, add water to adjust the solid content to 20% of the slightly yellow transparent liquid, and test its number average molecular weight to be 38,000.

[0043] The inorganic dust cleaner prepared in this example and the common cleaner purchased on the market (Comparative Example 2) were used to clean the dust on the exterior wall tiles. The cleaning effect was as follows: Figure 2The inorganic dust cleaner prepared in this embodiment can effectively clean the dust and dust accumulation on the exterior wall tiles, and has a good cleaning effect. The tiles are clean and free of dust after cleaning, while the ordinary cleaning agents purchased can only clean the dust on the surface of the tiles, but the dust accumulation attached to the tiles is still difficult to clean.

[0044] Example 3

[0045] The preparation method of the inorganic dust cleaning agent in this embodiment comprises the following steps: (1) preparation of base material: in a four-necked flask equipped with a thermometer and a stirrer, 401.44 g of propylene alcohol polyoxyethylene-polyoxypropylene ether (0.08 mol), 9.72 g (0.036 mol) of potassium persulfate and water are added and mixed and stirred evenly;

[0046] (2) Solution ① Preparation: Weigh 6.624 g (0.072 mol) of thioglycolic acid and 2.258 g (0.0058 mol) of Mohr's salt, add water to dissolve and stir evenly;

[0047] (3) Preparation of solution ②: Weigh 34 g (0.32 mol) of N-vinyl acetamide and 45.6 g (0.24 mol) of vinyl triethoxysilane, add water to dissolve and stir evenly;

[0048] (4) Heat the base material to 35° C. and simultaneously drip solutions ① and ② into the base material. Solution ① is dripped for 2.5 hours and solution ② is dripped for 2 hours. The total mass concentration of monomers A, B and C is controlled to be 40%. After the dripping is completed, keep the reaction warm for 1 hour, cool to room temperature, add ammonia water, adjust the pH to 7, add water to adjust the solid content to 20% of a slightly yellow transparent liquid, and test its number average molecular weight to be 26,000.

[0049] The inorganic dust cleaning agent prepared in this example and the common cleaning agent purchased on the market (Comparative Example 3) were used to clean the dust on the metal surface. The cleaning effect was as follows: Figure 3 As shown, it should be noted that the metal surface is not very smooth. The inorganic dust cleaner prepared in this embodiment can effectively clean the dust on the metal surface, with good cleaning effect, and the metal after cleaning is clean and bright, while the purchased ordinary cleaner can only clean the dust on the metal surface, but due to the fine bumps on the metal surface, dust particles remain in the small holes, forming gray stains.

[0050] Example 4

[0051] The preparation method of the inorganic dust cleaning agent in this embodiment comprises the following steps: (1) preparation of base material: in a four-necked flask equipped with a thermometer and a stirrer, 344.16 g of butenol polyoxyethylene-polyoxypropylene ether (0.08 mol), 5.76 g (0.064 mol) of tert-butyl hydroperoxide and water are added and mixed, and stirred evenly;

[0052] (2) Solution ① Preparation: Weigh 5.888 g (0.064 mol) of thioglycolic acid and 0.832 g (0.008 mol) of sodium bisulfite, add water to dissolve and stir evenly;

[0053] (3) Preparation of solution ②: Weigh 88.96 g (0.64 mol) of N-vinyl caprolactam and 15.2 g (0.08 mol) of vinyl triethoxysilane, add water to dissolve and stir evenly;

[0054] (4) Heat the base material to 40° C. and simultaneously drip solutions ① and ② into the base material. Solution ① is dripped for 3 hours and solution ② is dripped for 2.5 hours. The total mass concentration of monomers A, B and C is controlled to be 45%. After the dripping is completed, keep the reaction warm for 1 hour, cool to room temperature, add sodium hydroxide solution, adjust the pH to 7, add water to adjust the solid content to 25% of a slightly yellow transparent liquid, and test its number average molecular weight to be 22,000.

[0055] The inorganic dust cleaning agent prepared in this example and the common cleaning agent purchased on the market (Comparative Example 4) were used to clean the dust on the desktop. The cleaning effect was as follows: Figure 4 The inorganic dust cleaner prepared in this embodiment can effectively clean the dust on the desktop, and has a good cleaning effect. The desktop is clean and bright after cleaning, while the ordinary cleaner purchased can only clean the dust on the upper layer of the desktop, but it is still difficult to remove the dust accumulated in the pores of the desktop, thereby forming gray stains on the desktop, which cannot be removed even after repeated cleaning.

[0056] The inorganic dust cleaning agent prepared in this example and the common cleaning agent purchased on the market (Comparative Example 5) were used to clean the dust accumulated on the leaf surface of the plant. The cleaning effect was as follows: Figure 5 The inorganic dust cleaner prepared in this embodiment can effectively clean the dust on the leaf surface, and the cleaning effect is good. The leaf surface is clean and bright after cleaning, while the purchased ordinary cleaner can only clean the dust on the upper layer of the leaf surface, but there is still dust on the leaf surface, and the cleaning effect is poor.

Claims

1. A method for preparing an inorganic dust cleaning agent, characterized in that The following steps are involved: (1) Preparation of base material: Add unsaturated polyether monomer A and oxidant into a reaction kettle, add water to dissolve and stir evenly; (2) Solution ① Preparation: Weigh the thiol chain transfer agent and reducing agent, add water to dissolve and stir evenly; (3) Preparation of solution ②: weigh unsaturated amide monomer B and unsaturated silane monomer C, add water to dissolve and stir evenly; (4) The temperature of the bottom material in the reactor is raised to 35-55°C, and solutions ① and ② are added dropwise to the reactor at the same time. The addition time is 1-4 hours, and the reaction temperature is controlled at 35-60°C. The total mass concentration of monomers A, B and C is controlled to be 30-60%. After the addition is completed, the reaction is kept warm for 1-2 hours, cooled to room temperature, an alkaline compound is added to adjust the pH to 6.5-7.5, and water is added to adjust the solid content to 20-30%, thereby obtaining an inorganic dust cleaner; The molar ratio of the monomers A, B and C is 1:(2-9):(1-3); The monomer A is a block polyether macromonomer, and its general formula is: ； In the above general formula, R 1 is H or methyl, R 2 is H or methyl, A is CH2 or CH2CH2; x is an integer from 10 to 50, and y is an integer from 10 to 150.

2. The method for preparing the inorganic dust cleaning agent according to claim 1, characterized in that: The monomer A is one or a mixture of any proportion of two or more of allyl alcohol, butenol, isobutenol or isopentenol with ethylene oxide and propylene oxide.

3. The method for preparing the inorganic dust cleaning agent according to claim 1, characterized in that: The monomer B is one or a mixture of two or more of N-vinyl caprolactam, N,N-dimethylacrylamide, N,N-diethylacrylamide, isopropylacrylamide, N-vinylpyrrolidone, N-vinylacetamide, N-vinylformamide, and N-methyl-N-vinylacetamide.

4. The method for preparing the inorganic dust cleaning agent according to claim 1, characterized in that: The monomer C is one or a mixture of two or more of γ-methacryloxypropyltrimethoxysilane, vinyltrimethoxysilane and vinyltriethoxysilane.

5. The method for preparing the inorganic dust cleaning agent according to claim 1, characterized in that: The oxidant is one or a mixture of two of hydrogen peroxide, ammonium persulfate, potassium persulfate, tert-butyl hydroperoxide or cumene hydroperoxide in any proportion, and the amount of the oxidant is 1-8% of the total molar number of the three monomers A, B and C.

6. The method for preparing the inorganic dust cleaning agent according to claim 1, characterized in that: The mercaptan chain transfer agent is one or a mixture of any proportion of mercaptoacetic acid, mercaptopropionic acid and mercaptoethanol, and the amount of the chain transfer agent is 1-15% of the total molar number of the three monomers A, B and C.

7. The method for preparing the inorganic dust cleaning agent according to claim 1, characterized in that: The reducing agent is one of vitamin C, Rongalite, sodium bisulfite or Mohr's salt, or a mixture of two or more of them in any proportion, and the amount of the reducing agent is 0.1-2% of the total molar number of the three monomers A, B and C; the alkaline compound is one of ammonia water and alkali metal hydroxide, or a mixture of two or more of them in any proportion.

8. The method for preparing the inorganic dust cleaning agent according to claim 1, characterized in that: The number average molecular weight of the prepared inorganic dust cleaning agent is 20000-80000.

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